反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
Bring a mixture of trifluoro-methanesulfonic acid 4-{3-[4-(tert-butyl-diphenyl-silanyloxy)-cyclohexyl]-2-oxo-pyrrolidin-1-ylmethyl}-3,5-dichloro-phenyl ester (0.61 g, 0.84 mmol), 4-methoxycarbonylphenylboronic acid (0.18 g, 1 mmol), sodium carbonate (0.267 g, 2.52 mmol) in THF (15 mL) and water (5 mL) to 60° C. To the mixture at 60° C., add Pd(PPh3)4 (0.048 g, 0.04 mmol). Raise the reaction temperature to 80° C. and stir for 1 hour. Cool the reaction, dilute with ethyl acetate, and wash with water and brine. Dry the organic layer (Na2SO4), remove the solvent in vacuo to afford crude product, and purify on silica gel column with 25% ethyl acetate in hexanes to afford 0.56 g (93%) of the titled product. MS (m/z): 714 (M+).
WORKUP
后处理
- temperatureCool
- customthe reaction
- washwash with water and brine
- dry with materialDry the organic layer (Na2SO4)
- customremove the solvent in vacuo
- customto afford crude product
- custompurify on silica gel column with 25% ethyl acetate in hexanes