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ChemicalBook CAS DataBase List 4-Bromotriphenylamine
36809-26-4

4-Bromotriphenylamine synthesis

11synthesis methods
To a solution of triphenylamine(2.1 g, 8.16 mmol) in 40mL CCl4, NBS (1.6g,8.16 mmol) was added and the reaction mixture refluxed for 4 h under nitrogen (N2) atmosphere. During the reaction, a solid was formed, which conformed as succinimide. After filtering, the reaction mixture, filtrate was evaporated and recrystallized from ethanol to yield 4-Bromotriphenylamine 93%.
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Yield:36809-26-4 91%

Reaction Conditions:

with tri-tert-butyl phosphine;palladium diacetate;sodium t-butanolate in toluene at 115; for 10 h;Inert atmosphere;

Steps:

1.1
1) In a dry 500 mL three-necked flask, add 4-bromoaniline (17.20 g, 100 mmol) and bromobenzene (31.40 g, 200 mmol), toluene (200 mL) and sodium tert-butoxide (28.83 g, 300 mmol), and sonicate remove the air, under the protection of nitrogen,Add palladium acetate (0.07 g, 0.3 mmol) and tri-t-butylphosphine (0.18 g, 0.6 mmol) the reaction was heated under reflux at 115 ° C for 10 hours. The reaction was monitored by liquid phase. After cooling to room temperature,It was washed twice with water, separated, and the organic phase was dried over anhydrous magnesium sulfate, filtered, The filtrate was decolorized by adding activated carbon at 115 ° C for 30 minutes, hot filtration, and the filtrate was concentrated. After beating with ethanol twice, 29.50 g of intermediate a can be obtained with a yield of 91%.

References:

Wuhan Shang Sai Optoelectric Technology Co., Ltd.;Mu Guangyuan;Zhuang Shaoqing;Ren Chunting CN110590568, 2019, A Location in patent:Paragraph 0039-0042

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