反应 #6071

反应方程式

dimethyl maleate

phenyl vinyl sulfide

ethylaluminum dichloride

hexane

→

title compound

Dimethyl 3-phenylthiocyclobutane-1,2-dicarboxylate

溶剂

1,2-dichloroethane

methylene chloride

反应条件

后处理

1. 1
   洗涤The methylene chloride solution was washed three times with saturated aqueous ammonium chloride
2. 2
   干燥once with brine, dried over anhydrous sodium sulfate
3. 3
   过滤filtered
4. 4
   浓缩concentrated

实验过程

To a solution of dimethyl maleate (0.50 mL, 4 mmol) and phenyl vinyl sulfide (0.52 mL, 4 mmol) in 17 mL of 1,2-dichloroethane under nitrogen atmosphere, was added 1 equivalent (4 mL of a 1 M solution in hexane) of ethylaluminum dichloride. The resultant solution was heated at 85° C. for 18 h and then diluted with 75 mL of methylene chloride. The methylene chloride solution was washed three times with saturated aqueous ammonium chloride and once with brine, dried over anhydrous sodium sulfate, filtered and concentrated to give 0.98 g of the title compound; EI-MS, m/e (rel intensity): 280 (M+, 14), 136 (100).

来源