반응 #6071

반응 방정식

dimethyl maleate

phenyl vinyl sulfide

ethylaluminum dichloride

hexane

→

title compound

Dimethyl 3-phenylthiocyclobutane-1,2-dicarboxylate

용매

1,2-dichloroethane

methylene chloride

반응 조건

후처리

1. 1
   세척The methylene chloride solution was washed three times with saturated aqueous ammonium chloride
2. 2
   건조once with brine, dried over anhydrous sodium sulfate
3. 3
   여과filtered
4. 4
   농축concentrated

실험 절차

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).

출처