反应详情

温度

-30 °C

Butyl 3-(2-{[4-(methyloxy)phenyl]methyl}-3,6-dioxo-1,2,3,6-tetrahydro-4-pyridazinyl)propanoate (0.56 g, 1.56 mmol) was dissolved in dry THF (30 ml). The solution, under argon, was cooled to −30° C., and treated dropwise with a 1M solution of lithium aluminium hydride in THF (1.8 ml, 1.8 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. Chromatography of the residue, eluting with ethyl acetate, gave the product as a white solid (300 mg, 67%).

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. washChromatography of the residue, eluting with ethyl acetate