反应详情

温度

-30 °C

Butyl 3-(1-{[4-(methyloxy)phenyl]methyl}-3,6-dioxo-1,2,3,6-tetrahydro-4-pyridazinyl)propanoate (0.43 g, 1.19 mmol) was dissolved in dry THF (20 ml). The solution under argon was cooled to −30° C., treated dropwise with a 1M solution of lithium aluminium hydride in THF (1.4 ml, 1.4 mmol), allowed to warm gradually to 0° C. and stirred in an ice bath for 30 minutes. 2M Hydrochloric acid was added until the pH was 3 and the mixture was partitioned between water and ethyl acetate. The aqueous was re-extracted with ethyl acetate and the combined organic solution dried and evaporated. The resulting solid was triturated under ethyl acetate, filtered off, washed with ethyl acetate and dried under vacuum to give the product (241 mg, 70%).

1. temperatureto warm gradually to 0° C.
2. customthe mixture was partitioned between water and ethyl acetate
3. extractionThe aqueous was re-extracted with ethyl acetate
4. customthe combined organic solution dried
5. customevaporated
6. customThe resulting solid was triturated under ethyl acetate
7. filtrationfiltered off
8. washwashed with ethyl acetate
9. customdried under vacuum