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ChemicalBook CAS DataBase List 1-(4-BroMophenyl)-1,2,2-triphenylethylene
34699-28-0

1-(4-BroMophenyl)-1,2,2-triphenylethylene synthesis

10synthesis methods
-

Yield:34699-28-0 89%

Reaction Conditions:

Stage #1:Diphenylmethane;(4-bromophenyl)(phenyl)methanone with n-butyllithium in tetrahydrofuran for 1.33333 h;Inert atmosphere;Cooling with ice;
Stage #2:(4-bromophenyl)(phenyl)methanone in tetrahydrofuran at 20; for 12 h;

Steps:

3.1 (1) Synthesis of intermediate 1-bromo-4- (1,2,2-triphenylvinyl) benzene. (Si-Br)
16.7 mL (0.1 mol) of diphenylmethane and 300 ml of tetrahydrofuran (THF) were added to a solution of500ml three-necked flask, magnetic stirring and argon, ice salt bath 40min, to the three bottles by adding 54.5mL (0.12mol) n-butyl lithium solution, continue ice salt bath 40min, add 13.0555g4-bromobenzophenone(Bis (4-bromophenyl) methanone, 0.05),After the reaction was carried out at room temperature for 12 h, 250 ml of saturated ammonium chloride (NH4Cl) solution was added to the three-necked flask. After stirring for 10 min, the reaction solution was poured into a separatory funnel, the supernatant was taken and the water in the solution was adsorbed with 300 g of anhydrous sodium sulfate. And then heated to 110 ° C. After adding 5 g of p-toluenesulfonic acid, the mixture was refluxed for 12 hours. After the reaction was stopped, the reaction solution was dried and dried. The reaction mixture was heated to 110 ° C, The product was spin dried to dry the powder and the powder was dried in vacuo at 60 ° C for 24 h to give the white intermediate Si-Br in 89% yield.

References:

Sun Yat-sen University;Zhang, Yi;Liu, Yiwu;Xu, Jiarui;Wu, Xinhui;Shi, Jie;Liu, Siwei;Chi, Zhenguo CN104341311, 2016, B Location in patent:Paragraph 0057; 0058; 0059

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