HRID515849

反应详情

EQUATION

反应方程式

HRID 515849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction mixture was quenched with water at 0° C.
  2. additionpoured into saturated sodium bicarbonate (50 mL)
  3. extractionextracted with ethyl acetate (2×100 mL)
  4. washThe combined organic extracts were washed with brine (50 mL)
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated