1-(4-Bromophenyl)-2,2-bis(4-methoxyphenyl)-1-phenylethene synthesis

Yield: 57%

Reaction Conditions:

with pyridine;titanium tetrachloride;zinc in tetrahydrofuran at 0 - 70;Inert atmosphere;

Steps:

1.1 4,4'-(2-(4-bromophenyl)-2-phenylethene-1,1-diyl)bis(methoxybenzene) [1a]
The 24.2g (372mmol) of zinc powder was suspended in 250mL of tetrahydrofuran(THF) was added 1L three-neck flask, a magnetic stirred and purged with argon. Thesystem was reduced to 0 added dropwise 21mL (186mmol) of titanium tetrachloride wasadded dropwise at room temperature to complete the reaction system was returned after 30min, was heated in an oil bath and then raised to 70 °C , the reaction 3h. After again lowered to 70 °C, was added dropwise to 7.4g (93mmol) of pyridine, 200mL Afterdropping was dissolved tetrahydrofuran (THF) of 4,4'-dimethoxy-benzophenone 9g(37.2mmol) and 4-bromo benzophenone 12.6g (48.4mmol), after the completion of thedropwise addition heated at 70 ° C for 8 hours under an oil bath overnight. After completion of the reaction, the system was again cooled to 0 °C, was added200mL quenched with saturated sodium bicarbonate solution, diatomaceous earth, thefilter cake was washed with 200mL ethyl acetate and the filtrate was partitioned, theorganic phase by rotary evaporation, mixed with silica gel kind, by column to give 9.9 g of product, 57% yield

References:

Tianjin First Central Hospital;Nankai University;Liu Qian;Ni Xiang;Ding Dan;Gao Heqi CN108558788, 2018, A Location in patent:Paragraph 0025; 0028-0031