反应详情

A mixture of 3,4-dichlorobenzenethiol (1.15 ml), sodium 3-methoxycarbonyl-2-methylenepropionate (1.50 g), methanol (40 ml), and triton B (40% methanol solution, 5 drops) was refluxed for 20 hours. The reaction mixture was concentrated in vacuo. To the resulting residue was added a diluted hydrochloric acid, and a separated oil was extracted with diethyl ether. The organic layer was washed with water, dried over MgSO4, and evaporated at reduced pressure. The residue was purified by flash column chromatography on silica by eluting with chloroform/ethanol (10:1) to give 2.34 g of 3-(3,4-dichlorophenylthio)-2-methoxycarbonylmethylpropionic acid as an oil.

1. temperaturewas refluxed for 20 hours
2. concentrationThe reaction mixture was concentrated in vacuo
3. additionTo the resulting residue was added a diluted hydrochloric acid
4. extractiona separated oil was extracted with diethyl ether
5. washThe organic layer was washed with water
6. dry with materialdried over MgSO4
7. customevaporated at reduced pressure
8. customThe residue was purified by flash column chromatography on silica
9. washby eluting with chloroform/ethanol (10:1)