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
To toluene 4.0 mL suspension of methyl 2-(4-fluoroanilino)-4-iodobenzoate 0.40 g, 1,1′-bis(diphenylphosphino)ferrocene 0.072 g and tris(dibenzylideneacetone)dipalladium(0) 0.050 g were added triethylamine 0.30 mL and phenylmethanethiol 0.15 mL, and it was stirred under argon atmosphere at 80° C. for 2 hours. After the reaction mixture was cooled to room temperature, 1.0 mol/L hydrochloric acid and ethyl acetate were added to it. The organic layer was separated and collected,dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [Fuji SILYSIA Chemical Ltd., PSQ100B(spherical type), eluent, hexane:ethyl acetate=10:1] to give methyl 4-(benzylthio)-2-(4-fluoroanilino)benzoate 0.36 g of white solid.
WORKUP
后处理
- temperatureAfter the reaction mixture was cooled to room temperature
- customThe organic layer was separated
- customthe solvent was removed under reduced pressure