HRID1454934

反应详情

EQUATION

反应方程式

HRID 1454934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under argon, a solution of 3,5-dibromo-4-methylpyridine (intermediate 10.1, 2.51 g, 10 mmol) in anhydrous THF (100 ml) is reacted at a temperature of −100° C. with a solution of n-butyllithium in hexane (1.6N, 6.5 ml). The reaction mixture is stirred for 15 min and then dry ice is added. The temperature is kept for 15 min at −85° C., for 1 h 30 min at −78° C. and for 2 h at room temperature. Water is added. The solvents are evaporated under vacuum and the residue is purified, eluting on diol grafted silica with MeOH.

WORKUP

后处理

  1. waitThe temperature is kept for 15 min at −85° C., for 1 h 30 min at −78° C. and for 2 h at room temperature
  2. customThe solvents are evaporated under vacuum
  3. customthe residue is purified
  4. washeluting on diol