反应详情

温度

50 °C

NH3 gas is passed with cooling (max. 50° C.) through a solution of 99.7 g (0.6 mol) of methyl 2-chloro-3-oxo-valerate in 130 ml of formamide until the mixture takes up no more NH3 (about 1 h). The ammonia residues are removed by blowing out with nitrogen and applying a vacuum. The reaction solution is subsequently added dropwise to 450 ml of a 30% NaOMe solution in methanol at 50° C. Addition of a further 50 ml of formamide is followed by heating at 50° C. for 3 h. The volatile constituents are evaporated in vacuo, and subsequently the mixture is added to water and the pH is adjusted to 6 with HCl. Extraction with ethyl acetate and evaporation provide 91.2 g of crude product, which is recrystallized from cold acetone. Yield: 66.3 g (70%)

1. customThe ammonia residues are removed
2. additionThe reaction solution is subsequently added dropwise to 450 ml of a 30% NaOMe solution in methanol at 50° C
3. additionAddition of a further 50 ml of formamide
4. customThe volatile constituents are evaporated in vacuo
5. additionsubsequently the mixture is added to water
6. extractionExtraction
7. customwith ethyl acetate and evaporation