反应详情

A mixture of 2-naphthalenethiol (0.38 g), sodium 3-methoxycarbonyl-2-methylenepropionate (0.39 g), methanol (20 ml), and triton B (40% methanol solution, 10 drops) was refluxed for 12 hours. The reaction mixture was concentrated in vacuo, and the resulting residue was acidified with a dilute hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with water, and dried over MgSO4. The solvent was evaporated at reduced pressure, and the residue was purified by medium pressure liquid column chromatography on silica eluting with chloroform/methanol (20:1), and recrystallized from isopropyl ether to give 0.38 g of 2-methoxycarbonylmethyl-3-(2-naphthylthio)propionic acid.

1. temperaturewas refluxed for 12 hours
2. concentrationThe reaction mixture was concentrated in vacuo
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materialdried over MgSO4
6. customThe solvent was evaporated at reduced pressure
7. customthe residue was purified by medium pressure liquid column chromatography on silica eluting with chloroform/methanol (20:1)
8. customrecrystallized from isopropyl ether