Tag: M.W:200-300

98827-44-2. A heterogeneous catalyst is a catalyst that is present in a different phase than the reactants. Such catalysts generally function by furnishing an active surface upon which a reaction can occur. 98827-44-2, name is :Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, introduce a new downstream synthesis route as follows.

5.3 g of TNXK-3 and 20 ml of methanol were added to a reaction flask. Stir at room temperature. Separately add dimethyl sulfate 3.7 g methanol (5 ml) solution and 50% sodium hydroxide solution (5 ml). After the completion of the dropping, room temperature reaction 3 hours, cooling to 10 degrees, the water 50 ml dilution, use 10% hydrochloric acid to the PH is 3. Filtering, the filter cake after the water washing, drying, recrystallization with methanol, 60 degrees decompression drying, getting white solid 4.8 g, yield 86%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, and friends who are interested can also refer to it.

Reference£º
Patent; Jiangxi Yong Tong Technology Co., Ltd.; Liu Zhongchun; (13 pag.)CN107141308; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.92-30-8, name is :2-(Trifluoromethyl)-10H-phenothiazine, below Introduce a new synthetic route.. 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.

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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

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.92-30-8, name is :2-(Trifluoromethyl)-10H-phenothiazine, below Introduce a new synthetic route.. 92-30-8

Compound 13; 10-[3-(N-Boc-4-piperidyl)propyl]-2-trifluoromethylphenothiazine; To a stirred solution of 2-trifluoromethylphenothizine 1 (400 mg, 1.5 mmol), sodium hydride (100 mg, 2 mmol) in DME (10 mL) at 90 C was added N- Boc-4-(3-bromopropyl)piperidine 12 (380 mg, 1.24 mmol) dropwise under an atmosphere of argon. The reaction mixture was stirred for 12h at reflux. The reaction mixture was filtered and the filtrate was concentrated under vacuum. The residue was partitioned between ethyl acetate (25 mL) and brine (1OmL). The organic layer was dried over anhydrous sodium sulphate, filtered, and evaporated. The resulting residue was purified by silica gel column chromatography (8:2 hexane : ethyl acetate) on silica gel to give phenothiazine derivative 13 (425 mg, 70percent) as a solid. MS(ESI): m/z493 (M+H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand 2-(Trifluoromethyl)-10H-phenothiazine reaction routes.

Reference£º
Patent; IMMUNE CONTROL, INC.; WO2008/27521; (2008); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A heterogeneous catalyst is a catalyst that is present in a different phase than the reactants. Such catalysts generally function by furnishing an active surface upon which a reaction can occur. 92-30-8, name is :2-(Trifluoromethyl)-10H-phenothiazine, introduce a new downstream synthesis route as follows. 92-30-8

Compound 21; 10-(4-chlorobutyl)-2-trifluoromethylphenothiazine; To a stirred solution of 2-trifluoromethylphenothiazine 1 (4.Og, 15 mmol), sodium hydride (1.2g, 24 mmol) in dry toluene (40 mL), 1-bromo 4- chlorobutane (3.0 g, 17.6 mmol) was added. The reaction mixture was stirred for 18 hours at 110 C under an atmosphere of argon. The solution was cooled to room temperature and poured into an ice-water mixture. The crude product was extracted with ethyl acetate (3chi50mL) and the organic phase was dried over sodium sulphate. Final purification was performed by column chromatography (9: 1 hexane: ethyl acetate) on silica gel to give 21 (3.5 g, 65% ) as an oil., 92-30-8

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Reference£º
Patent; IMMUNE CONTROL, INC.; WO2008/27521; (2008); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

We know that the rate of many reactions can be accelerated by catalysts. A catalyst speeds up the rate of a reaction by lowering the activation energy; in addition, the catalyst is regenerated in the process. 188614-01-9, name is :Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate, below Introduce a new synthetic route.. 188614-01-9

Step 1. Borane-tetrahydrofuran complex solution (1 M in tetrahydrofuran, 45 mL, 45 mmol) was added at 0 C. to a suspension of methyl-3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate (2.00 g, 8.96 mmol) in tetrahydrofuran (20 mL). The ice bath was removed, the homogenous solution stirred at room temperature for 2 h, then excess reagent was destroyed by careful addition of methanol (42 mL) at 0 C. After evaporation of volatile material, the residue was taken up in 5% methanolic sulfuric acid solution (25 mL) and the solution was heated at reflux over 80 min. After cooling, the reaction mixture was partitioned between ethyl acetate and water, the organic layer was dried (MgSO4) and evaporated to produce 3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid methyl ester (1.79 g, 96%). Light yellow solid, MS (ISP)=210.1 (M+H)+., 188614-01-9

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand 188614-01-9 reaction routes.

Reference£º
Patent; Ackermann, Jean; Bleicher, Konrad; Ceccarelli, Simona M.; Chomienne, Odile; Mattei, Patrizio; Sander, Ulrike Obst; US2007/191603; (2007); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

An elementary termolecular reaction involves the simultaneous collision of three atoms, 188614-01-9, molecules, or ions. Here is a downstream synthesis route of the compound 188614-01-9, name is :Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate

A. 3-Oxo-3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid. To a solution of 3-oxo-3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid methyl ester (1.5 g, 6,7 mmol) in a THF/H2O mixture (1:1, 63 mL) was added 4 N LiOH (8.0 mL, 32 mmol) and the resulting solution was stirred at RT for 24 h. The solution was partially concentrated and diluted with H2O (50 mL). The solution was acidified using concentrated HCl and a solid precipitated. The solid was collected via filtration, washed with H2O and dried in vacuo to provide 0.79 g (60%) of the title compound as a white solid. MS (ESI): exact mass calculated for C9H7NO3S, 209.01; m/z found, 210.2 [M+H]+. 1H NMR (500 MHz, CD3OD): 7.65-7.61 (m, 2H), 7.40 (d, J=8.1, 1H), 3.48 (s, 2H).

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Reference£º
Patent; Allison, Brett D.; Gomez, Laurent; Grice, Cheryl A.; Hack, Michael D.; Morrow, Brian J.; Motley, S. Timothy; Santillan, Alejandro; Shaw, Karen J.; Schwarz, Kimberly L.; Tang, Liu Y.; Venkatesan, Hariharan; Wiener, John J. M.; US2006/223810; (2006); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

92-39-7. Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.92-39-7, name is :2-Chloro-10H-phenothiazine, below Introduce a new synthetic route.

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

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.92-39-7, name is :2-Chloro-10H-phenothiazine, below Introduce a new synthetic route.. 92-39-7

(1) Dehydration reaction: 2-chlorophenothiazine, cuprous cyanide, catalyst, quinoline, p-toluenesulfonyl chloride according to moleThe ratio is 1:1.25:0.15:5:0.1 is added to the reactor, and the temperature is raised to 120 C for dehydration reaction, the reaction is 1 hour, and the water is dehydrated to a moisture content of less than 0.1%;The catalyst is a mixture of sodium iodide and lithium iodide, and the molar ratio of sodium iodide to lithium iodide is 1:0.3;(2) Preparation of crude 2-cyanophenothiazine: the temperature of the reactor was raised to 230 C, and the reaction was carried out for 15 hours;(3) Separation of crude 2-cyanophenothiazine: the reactor temperature was lowered to 90 C, and 8 times was added to the reactor.The total amount of moles of the starting material is water, the solid is precipitated and filtered, and the product is extracted with ethyl acetate and concentrated to dryness to give a crude 2-cyanophenothiazine;(4) Purification of 2-cyanophenothiazine: a crude 2-cyanophenothiazine is placed in a mixed solvent of toluene and methanol,The volume ratio of toluene to methanol in the mixed solvent was 1:0.15, the temperature was raised to 120 C for 30 minutes, and the mixture was cooled to 20 C, and the precipitated solid was filtered to obtain 2-cyanophenothiazine.After testing, the yield of 2-cyanophenothiazine prepared in this example was 92.6%, and the purity of the product was 99.61%.The content of the amide was 0.03%.

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; Ningbo Jinuo Chemicals Co., Ltd.; Peng Zhigang; Yue Mingxin; Qu Qiangzheng; (8 pag.)CN105175355; (2018); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

272437-84-0. 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 272437-84-0, name is :3-Oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylic acid

To a solution of 3-oxo-3, 4-dihydro-2H-1, 4-benzothiazin-6- carboxylic acid (3.6 g, 17 mmol) in DMF (50 ML) were added WSC (3.8 g, 20 mmol), HOBt (3.1 g, 20 mmol) and 2.0 M dimethylamine-THF solution (12.5 ML, 25 mmol), and the mixture was stirred at room temperature for 12 hrs. Saturated aqueous sodium hydrogen carbonate was poured into the reaction solution and the mixture was extracted with ethyl acetate. The extract was washed with 1N hydrochloric acid and saturated brine, dried (MGS04) and concentrated under reduced pressure. The residue was crystallized from diisopropyl ether to give the title compound as pale yellow crystals (3.6 g, yield 90%). OH NMR (300 MHz, DMSO-D6) 8 ppm: 2.91 (br, 6 H), 3.49 (s, 2 H), 6. 96-7. 00 (m, 2 H), 7. 35 (d, J = 8. 4 Hz, 1 H)., 272437-84-0

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, 272437-84-0.

Reference£º
Patent; TAKEDA CHEMICAL INDUSTRIES, LTD.; WO2004/46107; (2004); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.3939-23-9, name is :3-Bromo-10H-phenothiazine. An updated downstream synthesis route of 3939-23-9 as follows.3939-23-9

To a stirred solution of 3-bromo-1OH-phenothiazine(1 8 g, 64.72 mmol) in DIVIF (100 mL) was added sodium hydride (3.8 g, 97.08 mmol) at 0 C in small portions and the reaction mixture was stirred at 0 C for 15 mins. To the reaction mixture was added 3-bromo chloropropane (12.2 g,77.66 mmol) at 0 C and stirring continued at room temperature for 1 h. The reaction wasquenched with aq.NH4C1 solution, extracted with EtOAc, organic layer is washed with brine, dried over anhydrous sodiumsulphate, and concentrated. The crude product (20 g) was as such taken for the next step without further purification: MS (ESI) m/z3 55 (M+2H).

According to the analysis of related databases, 3939-23-9, the application of this compound in the production field has become more and more popular.

Reference£º
Patent; BIOIMICS AB; KIRSEBOM, Leif; UPADHAYAYA, Ram Shankar; KETHIRI, Raghava Reddy; VIRTANEN, Anders; (308 pag.)WO2017/222466; (2017); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem