HRID12560

反应详情

EQUATION

反应方程式

HRID 12560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

General Procedure Q. To a suspension of NaH (20 mg, 0.80 mmol) in THF (2 ml) at 0° C. was added a solution of 1-(5,6-diphenyl-pyridin-2-yl)-ethanone oxime (Compound 80, 46 mg, 0.16 mmol) in THF (1 ml). After the mixture was stirred at the same temperature for 1 hour, MeI (140 mg, 0.99 mmol) was added and the solution was stirred overnight at room temperature. The reaction was quenched with water, and the products were extracted with ethyl acetate. The combined organic layers were washed with brine and dried over Na2SO4. The filtered solvent was concentrated in vacuo, and the residue was purified by silica gel chromatography (10% ethyl acetate in hexane) to give title compound as an oil.

WORKUP

后处理

  1. stirringthe solution was stirred overnight at room temperature
  2. customThe reaction was quenched with water
  3. extractionthe products were extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationThe filtered solvent was concentrated in vacuo
  7. customthe residue was purified by silica gel chromatography (10% ethyl acetate in hexane)