HRID1972154

反应详情

EQUATION

反应方程式

HRID 1972154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of sodium hydride (5.27 g, 209 mmol) in DMF (100 mL) was carefully charged with 5-(hydroxymethyl)-2,4-dimethylpyridin-3-ol hydrochloride (18 g, 95 mmol). The mixture stirred at ambient temperature for 2 hours. 2-chloro-4-nitropyridine (15 g, 95 mmol) was then added and the reaction stirred overnight at ambient temperature. The material was diluted with water and extracted with ethyl acetate. The organic layer was dried, and concentrated. Flash chromatography (dichloromethane/methanol 20:1) gave the title compound (19.8 g, 79%) as colorless oil.

WORKUP

后处理

  1. stirringthe reaction stirred overnight at ambient temperature
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was dried
  4. concentrationconcentrated