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
- 85 °C
PROCEDURE
实验过程
To a mixture of (E)-1-((3-bromothiophen-2-yl)methylene)-2-(diphenylmethylene)hydrazine (15 g, 40.6 mmol, including its Z isomer) and (diphenylmethylene)hydrazine (9.57 g, 48.7 mmol) in toluene (125 mL) was added palladium(II) acetate (0.120 g, 2.031 mmol), 1,1′-bis(diphenylphosphino)ferrocene (2.252 g, 4.06 mmol) and Cs2CO3 (26.5 g, 81 mmol). The reaction mixture was stirred at 85° C. for 14 hours and was subsequently diluted with toluene (25 mL) and filtered to remove undissolved solids. The filtrate was purified by flash column chromatography. The pure product fractions were evaporated to give the title compound (15.5 g, 79%). ESI-MS m/z [M+H]+ calc'd for C31H24N4S, 485. found, 485.
WORKUP
后处理
- filtrationfiltered
- customto remove undissolved solids
- customThe filtrate was purified by flash column chromatography
- customThe pure product fractions were evaporated