HRID886610

反应详情

EQUATION

反应方程式

HRID 886610 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(5-Bromopyridin-3-yl)acetic acid (500 mg, 2.31 mmol) was dissolved in dichloromethane (5 mL), treated with di-iso-propylamine (402.4 μL, 2.31 mmol) and cooled in an ice water bath. Pivaloyl chloride (284.7 μL, 2.31 mmol) was added and the mixture was stirred for 25 minutes. 2 M dimethylamine (1.73 mL, 3.46 mmol) was added and the reaction was stirred 15 h. The mixture was washed with saturated ammonium chloride (1×), saturated sodium bicarbonate (1×), and dried over sodium sulfate to yield 2-(5-bromopyridin-3-yl)-N,N-dimethylacetamide as a brown oil (445 mg, 79%). MS: m/z 562 (M+H+).

WORKUP

后处理

  1. temperaturecooled in an ice water bath
  2. stirringthe reaction was stirred 15 h
  3. washThe mixture was washed with saturated ammonium chloride (1×), saturated sodium bicarbonate (1×)
  4. dry with materialdried over sodium sulfate