反应详情

6.2 g (0.03 mole) of (S)-N-[1-(aminocarbonyl)propyl]-4-chlorobutanamide and 0.484 g (0.0015 mole) of tetrabutylammonium bromide are mixed in 45 ml of dichloromethane at 0° C. under a nitrogen atmosphere. 2.02 g (0.036 mole) of potassium hydroxide powder are added over 30 minutes, at such a rate that the temperature of the reaction mixture does not exceed +2° C. The mixture is then stirred for one hour, after which a further 0.1 g (0.0018 mole) of ground potassium hydroxide is added and stirring continued for 30 minutes at 0° C. The mixture is allowed to return to ambient temperature. The insoluble matter is filtered off and the filtrate is concentrated under reduced pressure. The residue obtained is recrystallized from 40 ml of ethyl acetate in the presence of 1.9 g of 0,4 nm molecular sieve. The latter is removed by hot filtration to give 3.10 g of (S)-alpha-ethyl-2-oxo-1-pyrrolidineacetamide.

1. customdoes not exceed +2° C
2. stirringstirring
3. waitcontinued for 30 minutes at 0° C
4. customto return to ambient temperature
5. filtrationThe insoluble matter is filtered off
6. concentrationthe filtrate is concentrated under reduced pressure
7. customThe residue obtained
8. customis recrystallized from 40 ml of ethyl acetate in the presence of 1.9 g of 0,4 nm molecular sieve
9. customThe latter is removed by hot filtration