HRID1027702

反应详情

EQUATION

反应方程式

HRID 1027702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Oxalyl chloride (1.45 g, 11.1 mmol) was added to a suspension of 5-Bromo-pyrimidine-2-carboxylic acid (1.5 g, 7.4 mmol) in dichloromethane (50 ml) at room temperature followed by 1-2 drop of dimethylformamide. The reaction mixture was stirred under nitrogen for 2 hours LCMS in methanol indicated the presence of the methyl ester and some acid. Dimethylformamide (0.2 ml) was added to the reaction mixture and all of the acid dissolved after 30 minutes. LCMS showed corresponding methyl ester and no starting material peak was observed. The solvent was removed and dried in vacuo to afford the crude 5-Bromo-pyrimidine-2-carbonyl chloride (1.6 g).

WORKUP

后处理

  1. dissolutionall of the acid dissolved after 30 minutes
  2. customThe solvent was removed
  3. customdried in vacuo