New learning discoveries about 3939-23-9

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

3939-23-9, 3-Bromo-10H-phenothiazine is a thiazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Compound 1 was synthesized by the modification of the published method [18]. Sodium hydride(2.2 g, 53.9 mmol) was stirred with 3-bromo-10H-phenothiazine (10.0 g, 35.9 mmol, dissolved in dryDMF) for 30 min. Bromoethane (4.7 g, 43.1 mmol) was then added to the mixture and stirred for 10 hat room temperature in dark environment. After the reaction completed, water was added to react theremaining sodium hydride. White solid was precipitated and collected by vacuum filtration. The solidwas first washed with small amount of EA and then washed with n-hexane. 1H NMR (400 MHz,acetone-d6) 7.34 (dd, J = 8.7, 2.3 Hz, 1H), 7.28 (d, J = 2.3 Hz, 1H), 7.25-7.19 (m, 1H), 7.15 (dd, J = 7.6,1.5 Hz, 1H), 7.04 (dd, J = 8.3, 1.2 Hz, 1H), 6.99 (d, J = 1.2 Hz, 0H), 6.97 (s, 1H), 6.95 (s, 1H), 3.99 (q,J = 6.9 Hz, 2H), 1.38 (t, J = 6.9 Hz, 3H).

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

Reference£º
Article; Lao, Hio Kuan; Tan, Jingyun; Wang, Chunfei; Zhang, Xuanjun; Molecules; vol. 24; 19; (2019);,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Simple exploration of 3939-23-9

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3939-23-9,3-Bromo-10H-phenothiazine,as a common compound, the synthetic route is as follows.

In a 250 ml three-necked flask, 0.01 mol of raw material A1, 0.012 mol of raw material B1, 150 ml of toluene were added under a nitrogen atmosphere, and the mixture was stirred and mixed.Then, 0.03 mol of sodium t-butoxide, 5 ¡Á 10 -5 mol of Pd 2 (dba) 3, 5 ¡Á 10 -5 mol of tri-tert-butylphosphine was added, and the mixture was heated to 105 C, and refluxed for 24 hours.The sampling point plate shows that no raw material A1 remains, the reaction is complete; it is naturally cooled to room temperature, filtered, and the filtrate is steamed to a non-fraction (-0.09 MPa, 85 C) under reduced pressure, and passed through a neutral silica gel column to obtain an intermediate B1.HPLC purity 99.2%, yield 75.2%;

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Tang Dandan; Zhang Zhaochao; Li Chong; Zhang Xiaoqing; (44 pag.)CN108218853; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Some tips on 3939-23-9

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

3939-23-9, 3-Bromo-10H-phenothiazine is a thiazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2, under the protection of nitrogen will be prepared in step 1 aromatic diamine and phenothiazine derivatives according to 1:1 molar ratio was added to toluene, while adding potassium tert-butyl alcohol and palladium acetate as a catalyst,The reaction was heated to 80 C for 3 hours and then cooled to room temperature. The reaction was filtered,The filtrate was washed with dichloromethane and then the solvent was evaporated to dryness. The crude product was repeatedly washed with methanol and acetone,The product is obtained after purification by column chromatography.

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Guo Jianhua; (12 pag.)CN106831645; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Simple exploration of 3939-23-9

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3939-23-9,3-Bromo-10H-phenothiazine,as a common compound, the synthetic route is as follows.

In a nitrogen-flushed 250 mL round-bottom flask with a magnetic stir bar and septum 3-bromo-10H-phenothiazine (4.95 g, 17.8 mmol) was dissolved in dry THF (50 mL) under nitrogen. The colorless solution was deaerated by a constant stream of nitrogen through a syringe for 10 min and cooled to 0 C (ice bath/water). Potassium tert-butanolate (2.40 g, 21.4 mmol) was added to the reaction mixture under nitrogen and the reaction mixture was allowed to come to room temperature and then stirred for 1 h. To this solution 1-bromo hexane (3.00 mL, 21.4 mmol) was slowly added by syringe and stirring at room temp was continued for 16 h. The solvents were removed in vacuo and the residue was adsorbed onto celiteand purified by chromatography on silica gel (n-hexane) to give 5.83 g (90%) of 3-bromo-10-hexyl-10H-phenothiazine (1a) as a yellow resin, Rf (n-hexane) = 0.43. The NMR spectra were in excellent agreement with the literature. 1H NMR (300 MHz, acetone-d6): delta = 0.84 (t, 3J = 7.1 Hz, 3 H), 1.23-1.33 (m, 4 H), 1.44 (dt, 3J = 7.2 Hz, 3J = 6.8 Hz, 2 H), 1.77 (dt, 3J = 7.5 Hz, 3J = 7.5 Hz, 2 H), 3.92 (t, 3J = 7.0 Hz, 2 H), 6.95 (d, 3J = 8.7 Hz, 2 H), 7.03 (dd, 3J = 8.2 Hz, 4J = 0.9 Hz, 1 H), 7.14 (dd, 3J = 7.6 Hz, 4J = 1.4 Hz, 1 H), 7.21 (ddd, 3J = 8.2 Hz, 3J = 7.3 Hz, 4J = 1.6 Hz, 1 H), 7.27 (d, 4J = 2.2 Hz, 1 H), 7.32 (dd, 3J = 8.6 Hz, 4J = 2.3 Hz, 1 H). -13C NMR (75 MHz, acetone-d6): delta = 14.2 (CH3), 23.2 (CH2), 27.0 (CH2), 27.4 (CH2), 32.1 (CH2), 47.9 (CH2), 114.7 (Cquat), 116.9 (CH), 118.1 (CH), 123.6 (CH), 124.7 (Cquat), 128.1 (Cquat), 128.1 (CH), 128.6 (CH), 130.0 (CH), 130.9 (CH), 145.7 (Cquat), 145.9 (Cquat).

The synthetic route of 3939-23-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Urselmann, Dominik; Deilhof, Konstantin; Mayer, Bernhard; Mueller, Thomas J. J.; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 2055 – 2064;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

New learning discoveries about 3939-23-9

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

3939-23-9, 3-Bromo-10H-phenothiazine is a thiazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

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%.

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

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

 

Brief introduction of 3939-23-9

As the paragraph descriping shows that 3939-23-9 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3939-23-9,3-Bromo-10H-phenothiazine,as a common compound, the synthetic route is as follows.

Step 2, 132 mmol of 9-BBN was dissolved in THF at 0 C, 44 mmol of 1-2, Stirring for 15min, warming to 35 degrees Celsius, reaction 3h, and then transferred to the mixture containing 5-1 66mmoltetrakis(triphenylphosphine)palladium 0.88 mmol, sodium carbonate 132 mmol in toluene: ethanol: water = 4: 1: 1, and the temperature was raised to reflux temperature reaction24h. The crude product was passed through a silica gel column to give the product 20 mmol, 5-2.

As the paragraph descriping shows that 3939-23-9 is playing an increasingly important role.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Sun Keyi; Cai Hui; (31 pag.)CN106946934; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Downstream synthetic route of 3939-23-9

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3939-23-9,3-Bromo-10H-phenothiazine,as a common compound, the synthetic route is as follows.

2, under nitrogen protection will be prepared in step 1 p-phenylenediamine and phenothiazine derivatives according to 1:1 molar ratio was added to toluene, while adding potassium tert-butyl alcohol and palladium acetate as a catalyst,The reaction was heated to 80 C for 3 hours and then cooled to room temperature. The reaction was filtered,The filtrate was washed with dichloromethane and then the solvent was evaporated to dryness. The crude product was repeatedly washed with methanol and acetone,The product is obtained after purification by column chromatography.

3939-23-9 3-Bromo-10H-phenothiazine 283308, athiazines compound, is more and more widely used in various.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Guo Jianhua; (12 pag.)CN106831645; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem