反应详情

An ammonium salt (102 g) of dithiocarbamic acid was dissolved in ethanol (700 mL), and a solution of 4-chloro-3-oxobutanoic acid ethyl ester (152 g) in ethanol (200 mL) was added dropwise under ice-cooling over 30 min. The temperature was gradually raised, and the mixture was heated under reflux for 2 hr. The reaction solution was concentrated under reduced pressure, water (1 L) was added thereto, and the precipitated solid was collected by filtration. This solid was dissolved in ethyl acetate (4 L), and the mixture was washed with water (2 L) and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether (500 mL) was added to the obtained solid, and the solid was washed by suspending and collected by filtration to give the title compound (165 g) as a slightly yellow solid.

1. temperaturecooling over 30 min
2. temperatureThe temperature was gradually raised
3. temperaturethe mixture was heated
4. temperatureunder reflux for 2 hr
5. concentrationThe reaction solution was concentrated under reduced pressure, water (1 L)
6. additionwas added
7. filtrationthe precipitated solid was collected by filtration
8. dissolutionThis solid was dissolved in ethyl acetate (4 L)
9. washthe mixture was washed with water (2 L)
10. dry with materialdried over anhydrous magnesium sulfate
11. customThe solvent was evaporated under reduced pressure
12. additionDiethyl ether (500 mL) was added to the obtained solid
13. washthe solid was washed
14. filtrationcollected by filtration