HRID1752874

反应详情

EQUATION

反应方程式

HRID 1752874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Bromo-3-formyl-4-methoxybenzoic acid (480 mg, 1.84 mmol) was dissolved in anhydrous tetrahydrofuran (20 mL) and the solution was flushed with dry nitrogen for 5 minutes. Oxalyl chloride (1.2 mL, 2.4 mmol, 1.3 eq) was added slowly to the solution while vigorous stirring and then a catalytic amount of dry dimethylformamide was added. The mixture was stirred for 1 hour and then concentrated by rotary evaporation and dried on high vacuum to give 5-bromo-3-formyl-4-methoxybenzoyl chloride (501 mg) as yellow crystals.

WORKUP

后处理

  1. customthe solution was flushed with dry nitrogen for 5 minutes
  2. stirringThe mixture was stirred for 1 hour
  3. concentrationconcentrated by rotary evaporation
  4. customdried on high vacuum