HRID2221441

反应详情

EQUATION

反应方程式

HRID 2221441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-methyl-benzofuran-2-carboxylic acid (0.98 g, 5.6 mmol) and catalytic amount of DMF (5 drops) in THF (25 ml) was added oxalyl chloride (0.53 ml, 6.1 mmol). After stirring the solution for 1 h at room temperature, methanol (20 ml) and TEA (7.0 ml) were added. The reaction mixture was stirred overnight at room temperature, then concentrated and dissolved in ethyl acetate (100 ml) and washed with aqueous sodium bicarbonate solution (100 ml). The organic layer was dried over sodium sulfate and concentrated to provide crude methyl 3-methylbenzofuran-2-carboxylate (1.0 g, 5.3 mmol) as a tan solid, which was used without further purification.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred overnight at room temperature
  2. concentrationconcentrated
  3. dissolutiondissolved in ethyl acetate (100 ml)
  4. washwashed with aqueous sodium bicarbonate solution (100 ml)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated