Month: November 2020

92-30-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.92-30-8,2-(Trifluoromethyl)-10H-phenothiazine, it is a common compound, a new synthetic route is introduced below.

After dissolving 2-(trifluoromethyl)-10H-phenothiazine (2.0 g, 7.48 mmol) in N,N-dimethylformamide (2 mL), 60% sodium hydride (149.70 mg, 3.74 mmol) and 1-bromo-4-chlorobutane (1.16 mL, 10.10 mmol) were added at 0 C. The reactants were heated at 100 C. for 12 hours under reflux. After the reaction was completed, the reaction solution was extracted with ethyl acetate and the organic layer was dried with magnesium sulfate, filtered under reduced pressure and then concentrated under reduced pressure. The target compound (1.52 g) was obtained with a yield of 56.72% by separating the residue by chromatography (ethyl acetate/n-hexane=1/20). 1H NMR (400 MHz, CDCl3): delta 1.89-2.00 (4H, m, 2CH2), 3.40 (1H, t, J=6.02 Hz, CH), 3.54 (1H, t, 6.18 Hz, CH), 3.94 (2H, t, 6.02 Hz, CH2), 6.89 (1H, d, J=8.12 Hz, CH), 6.96 (1H, t, 7.44 Hz, CH) 7.03 (1H, s, CH), 7.13-7.17 (2H, m, 2CH), 7.21 (2H, t, 8.16 Hz, 2CH).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 92-30-8, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; Korea Institute of Science and Technology; Roh, Eun Joo; Jeon, Bo Ra Mi; Lee, Chang Joon; Hong, Jin Pyo; Jeong, Joo Yeon; Kang, Sang Soo; (28 pag.)US10035795; (2018); B1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

92-39-7,Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2-Chloro-10H-phenothiazine,92-39-7, This compound has unique chemical properties. The synthetic route is as follows.

Step: Step 1, the reaction system azeotropic water removal: To the reaction kettle with argon gas was added 50 kg of N-methylpyrrolidone at room temperature, 2-chlorophenothiazine 50 kg, cuprous cyanide 23 kg, lithium iodide 0.23 kg, potassium iodide 3.55 kg and cyclohexane 25 kg, Stirring up to 85C , boiling a total of boiling water, about 40min, measured water 0.04wt.% (Moisture ? 0.05wt.%). Step 2: Preparation of 2-cyanophenothiazine by refluxing reaction: The reaction system after the removal of water continued to warm to 112 C, Atmospheric distillation distillation system in the cyclohexane, cyclohexane can be recycled recycling, Continue to heat up to the reflux state (T = 218 ), insulation reaction 10h, To obtain a reaction product; Step 3, the reaction product after treatment and extraction: After the reaction, the temperature was lowered to 75 C, To the reaction system was added sodium thiosulfate solution (sodium thiosulfate 33 kg and water 250 kg mixed dissolved) Stirring for 2h, cooling to 5 , filtering, the first filter cake and the first filtrate, The first filter cake was dried at 90 C to a moisture content of ? 4 wt.%. The first filter cake was extracted with acetone, The dried cake and acetone 700L, heated to reflux 30min, down to 50 , The second filter cake and the second filtrate were filtered and the second filtrate was concentrated at atmospheric pressure to give 500 L of acetone to give a concentrate, The concentrated liquid for low temperature precipitation, the specific process is to concentrate the solution to 0 , filtration, Dried 2-cyanophenothiazine crude 45kg, 98% purity, amide impurity 0.9%.Step 4: Purification of crude 2-cyanophenothiazine: 2-cyanophenothiazine crude 45kg and acetone 36kg heated to reflux, reflux insulation 30min. Cooled to 0 C, filtered and dried to give 4-cyano phenothiazine 43.2 kg, purity ?99% Amide impurities ? 0.1%, yield: 90.0%This example gives an industrial preparation method of an environment-friendly 2-cyanophenothiazine, The method of other processes and implementation Example 1 is the same, the difference is only: In the third step, the mass of the dried first filter cake and the ratio of the second organic solvent acetone used in the first filter cake Was adjusted to 1:15 from 1: 8 of Example 1. The yield of 2-cyanophenothiazine was 90.2% based on 2-chlorophenothiazine

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 92-39-7.

Reference£º
Patent; Xi’an Caijing Optoelectric Technology Co., Ltd.; Gao Aiai; Zhao Qunxing; Zhou Bugao; Fan Jia; Bie Guojun; Yan Xiaoliang; Lan Aihu; Guo Chuang; Li Jian; Xu Lei; Zhang Weijie; Wang Li; (11 pag.)CN106946811; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Adding a certain compound to certain chemical reactions, such as: 37441-50-2,1,2-Thiazinane 1,1-dioxide, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 37441-50-2,37441-50-2

A stirred mixture of methyl 6-BROMO-3-HYDROXYPYRIDINE-2-CARBOXYLATE (6.15 g, 26.5 mmol), 8-sultam (described in WO 02/30931-A2, Merck & Co. , Inc. , 2002) (3. 98 g, 29.4 mmol) and copper (I) oxide (5.75 g, 40.2 mmol) in anhydrous pyridine (100 mL) was heated at 130 C, under argon, for 6 h. The mixture was cooled, and the pyridine removed under reduced pressure. The residue was treated with CH2C12 (400 mL) and EDTA (0.35 M in H20, 300 ML, 105 mmol) and air was bubbled into the mixture for 18 h. The mixture was filtered through a pad of celite and the aqueous layer was saturated with solid NACI and extracted with CH2CLZ (4 x 250 mL). The combined organic extracts were dried (NA2S04), filtered, and concentrated in vacuo to afford a crude oil. The oil was dissolved in MEOH (400 mL) and conc. H2S04 (2 ML) and heated to reflux for 18 h, then allowed to cool to ambient temperature. Most of the solvent was removed in vacuo and the residual mixture was partitioned between CHZCLX (400 mL) and saturated NAHCO3 (400 mL). The aqueous layer was extracted further with CH2Cl2 (2 x 250 mL) and the combined organic extracts were dried (NA2S04), filtered, and concentrated in vacuo to afford a crude sample of the product. This crude product was partially purified by silica gel chromatography, eluting with a gradient of CH2C12 : MEOH-100 : 0 to 95: 5 to give a yellow solid that was crystallized from MEOH to afford the title compound as a pale yellow solid of sufficient purity for use in the next step. MS: FALZ = 287 (M + 1).

According to the analysis of related databases, 37441-50-2, the application of this compound in the production field has become more and more popular.

Reference£º
Patent; MERCK & CO., INC.; WO2005/9962; (2005); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 188614-01-9,Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate, as follows.188614-01-9

3-Oxo-3, 4-dihydro-2H-benzo [1, 4] thiazine-6-carboxylic acid methyl ester (6.74 g) was suspended in tetrahydrofuran (100 ml) and 2M sodium hydroxide [(30] ml) was added followed by water (20 ml). The solution was stirred for 2.5 hours, evaporated to half volume and acidified with 2M hydrochloric acid. The product was collected, washed with water and dried in vacuo, to give a white solid (6.2 g). MS (-ve ion electrospray) [L} L/Z] 208 (M-H)-

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate, We look forward to the emergence of more reaction modes in the future.

Reference£º
Patent; GLAXO GROUP LIMITED; WO2004/2992; (2004); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 37441-50-2,37441-50-2

Intermediate 524-Fluoro- 2-(l,l-dioxo-llambda6-[l,2]thiazinan-2-yl)benzonitrile: To a solution of l,l-dioxo[l,2]thiazinane (8.84 g, 65.4 mmol) in DMF (20 mL) and THF (10 mL) was added portion-wise sodium hydride (1.65 g, 65.5 mmol, 95%). After stirring for 30 min, 2,4-difluorobenzonitrile (10.0 g, 72 mmol) was added and the mixture was stirred at 90 C for 2.5 h. The mixture was cooled and concentrated and the residue was purified by flash chromatography eluting with 0%-l 0% EtOAc/hexane to give the title compound as white needles (1.37 g, 8% yield). 1H-NMR (500 MHz, CDCl3) delta: 7.70 (IH, dd, J= 8.8, 5.8 Hz), 7.30 (IH, dd, J= 8.8, 2.4 Hz), 7.15-7.12 (IH, m), 3.72 (2H, t, J= 5.3 Hz), 3.33 (2H, t, J= 6.1 Hz), 2.40-2.35 (2H, m), 2.05-2.01 (2H, m). LCMS [M+H]+ calcd for C11H12N2FO2S: 255.06; found: 255.19.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 37441-50-2.

Reference£º
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/58646; (2007); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 92-30-8,2-(Trifluoromethyl)-10H-phenothiazine, as follows.92-30-8

To a mixture of 2-(trifluoromethyl)-l0i7-phenothiazine (5.0 g, 18.726 mmol) and NaH (0.674 g, 28.09 mmol) in DMF (50 mL) was added 2-(bromomethyl)oxirane (3.8 g, 28.09 mmol) at 0 C. The mixture was allowed to slowly warm to rt and was stirred at room temperature overnight. Then the mixture was added to water (100 mL) and extracted with EtOAc (100 mL x 3). The combined organic layers were washed with brine (30 mL), dried over sodium sulfate, and concentrated to dryness. The residue was purified by column chromatography on silica gel (PE/EtOAc = 8/1) to afford compound 2-1 (4.5 g, 75% yield) as a white solid. ‘H NMR (400 MHz, Patent; CAMP4 THERAPEUTICS CORPORATION; BUMCROT, David, A.; SEHGAL, Alfica; HERTZOG, Donald L.; (172 pag.)WO2019/195789; (2019); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.92-30-8,A new synthetic method of this compound is introduced below.92-30-8

II-4 (20g, 75mmol) a 100mL reaction flask was added DMF (60mL) was stirred and dissolved, was added potassium carbonate (15.5g, 113mmol), stirred at 60¡ãC , portionwise Intermediate III-5 (17.5g , 79mmol), the reaction after 1h, TLC analysis showed completion of the reaction (developing solvent, ethyl acetate: petroleum ether = 1: 3). The reaction solution was poured into 200ml cold water, with stirring, solid precipitated out.Filter cake was washed with water, and dried to give brown crude solid.The crude product was recrystallized from ethanol to give slightly yellow solid 30.0g. Purity 98.8percent (HPLC normalization method), a yield of 88.3percent.ESI-MS ([M + H] +): 453.0.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 2-(Trifluoromethyl)-10H-phenothiazine.

Reference£º
Patent; Tianjin Pharmaceutical Institute Co., Ltd.; Liu Ying; Liu Dengke; Mu Shuai; Yue Nan; Gong Min; Zhi Shuang; Liu Changxiao; (25 pag.)CN104230848; (2017); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

92-30-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.92-30-8,2-(Trifluoromethyl)-10H-phenothiazine, it is a common compound, a new synthetic route is introduced below.

General procedure: In an air atmosphere, 2-phenylindole 1a (0.60 mmol), phenothiazine 2a (0.30 mmol),10mol% cuprous bromide and DMF (2mL) were added to the Schlenk reaction tube in sequence.In a constant temperature heating magnetic stirrer, the reaction was stirred at room temperature for 24 hours.After the reaction was completed, it was quenched with distilled water, extracted with ethyl acetate (3 ¡Á 20 mL), and the organic layers were combined.After drying over anhydrous sodium sulfate and spinning the organic phase, The crude product by column chromatography to give the pure product 3a (103.1 mg, 88%).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 92-30-8, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; Henan Normal University; Zhao Peizheng; Wang Ke; Liu Jianming; Wang Zhixian; Shao Huibin; Yue Yuanyuan; (9 pag.)CN110407830; (2019); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.3939-23-9,3-Bromo-10H-phenothiazine, it is a common compound, a new synthetic route is introduced below.3939-23-9

Tri-tert-butylphosphine (4.4 mL of a 1.0 M solution in toluene, 1.48 g, 0.05 mmol), palladium acetate (0.4 g,1.83 mmol) and sodium tert-butoxide (52.7 g, 549 mmol) were added to 2-6-a (20.423 g, 73.42 mmol) and 2-6-c(11.53 g, 73.42 mmol) a solution in degassed toluene (500 mL), and the mixture was warmed under reflux for 2 hr.The reaction mixture was cooled to room temperature, diluted with toluene and filtered over EtOAc. Dilute the filtrate with water and use aThe benzene was extracted and the organic phases were combined and evaporated under vacuum. The residue was passed through silica gel (heptane / dichloromethane)Filtration was carried out and crystallized from isopropanol. Obtaining 2-6-b 19.51 g, yield 75%; the resulting bromide 2-6-b(7.89 g, 20 mmol), pinacol borate (6.22 g, 24 mmol), 1,1′-bis(diphenylphosphino)-ferrocene-palladium dichloride(II) dichloromethane complex (0.49 g, 0.6 mmol), potassium acetate (5.90 g, 60 mmol) and 79 ml of toluene were reacted under refluxAfter 16 hours, cool, add 26 ml of water and stir for 30 minutes.The organic phase is separated and filtered through a short bed of diatomaceous earth, followed by organicThe solvent was distilled off and the crude product was recrystallized from heptane / toluene.The compound 2-6 was obtained in an amount of 6.58 g, yield 82%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 3939-23-9, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Zhang Hong; Cai Hui; (36 pag.)CN108530418; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Adding a certain compound to certain chemical reactions, such as: 98827-44-2,Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 98827-44-2,98827-44-2

EXAMPLE 6 A solution of 4-hydroxy-3-methoxycarbonyl-2H-thieno-[2,3-e]-1,2-thiazine 1,1-dioxide (0.7 g) and 2-aminotropone (0.341 g) in xylene (7 ml) was refluxed for 21 hours and the reaction mixture was allowed to stand at ambient temperature. The crystalline precipitates were collected by filtration, washed with toluene and recrystallized from tetrahydrofuran to give 4-hydroxy-N-(1-oxo-2,4,6cycloheptatrien-2-yl)-2H-thieno[2,3-e]-1,2-thiazine-3-carboxamide 1,1-dioxide (0.47 g). mp: 230 C. (dec.). IR (Nujol): 3260, 1550, 1500, 1450, 1400, 1340, 1180 cm-1 NMR (DMSO-d6, delta): 7.00-7.47 (5H, m), 7.57 (1H, d, J=5 Hz), 8.17 (1H, d, J=5 Hz), 8.89 (1H, d, J=9 Hz), 10.53 (1H, brs).

According to the analysis of related databases, 98827-44-2, the application of this compound in the production field has become more and more popular.

Reference£º
Patent; Fujisawa Pharmaceutical Co., Ltd.; US4563453; (1986); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem