反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of methyl 2-(3-(6-(1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)cyclopropanecarboxamido)-3-methylpyridin-2-yl)-5-methyl-2-oxopyridin-1(2H)-yl)acetate (17 mg, 0.034 mmol) in THF (1.6 mL) was added NaBH4 (7 mg, 0.17 mmol) and stirred at 50° C. for 3 hours and 15 minutes. The reaction was filtered using ethyl acetate and the solvent was evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel (0-100% ethyl acetate in hexane) to yield 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)-N-(6-(1-(2-hydroxyethyl)-5-methyl-2-oxo-1,2-dihydropyridin-3-yl)-5-methylpyridin-2-yl)cyclopropanecarboxamide as a white solid (5.5 g, 33.6%). ESI-MS m/z calc. 483.46. found 484.5 (M+1)+, retention time 1.49 minutes
WORKUP
后处理
- filtrationThe reaction was filtered
- customthe solvent was evaporated under reduced pressure
- customThe crude product was purified by column chromatography on silica gel (0-100% ethyl acetate in hexane)