HRID531242

反应详情

EQUATION

反应方程式

HRID 531242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 0° C. solution of (5-bromo-2-chloropyridin-4-yl)methanol (1.96 g, 8.81 mmol) in CH2Cl2 (25 mL) was treated with triethylamine (2.456 ml, 17.62 mmol) and methanesulfonyl chloride (0.824 ml, 10.57 mmol). The reaction was stirred at room temperature for 1 hour. The reaction was diluted with additional CH2Cl2, then washed with aqueous NaHCO3, followed by brine. The organic was dried over sodium sulfate, filtered and the filtrate evaporated. The crude was purified by silica gel chromatography to give the titled compound. 1H NMR (CDCl3, 500 MHz): δ 8.50 (s, 1H), 7.47 (s, 1H), 5.24 (s, 2H), 3.16 (s, 3H).

WORKUP

后处理

  1. washwashed with aqueous NaHCO3
  2. dry with materialThe organic was dried over sodium sulfate
  3. filtrationfiltered
  4. customthe filtrate evaporated
  5. customThe crude was purified by silica gel chromatography