HRID1192519
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of 1-{4-chloro-6-[(1E)-3,3-diethyltriaz-1-en-1-yl]-5-ethynyl-3′-fluorobiphenyl-2-yl}ethanone (2.3 g, 6.1 mmol) in methanol (38 mL) at 0° C. was treated with sodium borohydride (0.46 g, 12 mmol) in two portions and stirred at 0° C. for 30 minutes. The reaction mixture was quenched with water at 0° C., poured into saturated sodium bicarbonate (50 mL), and extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with brine (50 mL), dried with sodium sulfate, filtered, and concentrated to give the desired product (quantitative). This material was used without further purification. LCMS for C20H22ClFN3O (M+H)+: m/z=374.1; Found: 373.9.
WORKUP
后处理
- customThe reaction mixture was quenched with water at 0° C.
- additionpoured into saturated sodium bicarbonate (50 mL)
- extractionextracted with ethyl acetate (2×100 mL)
- washThe combined organic extracts were washed with brine (50 mL)
- dry with materialdried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated