HRID1403375

反应详情

EQUATION

反应方程式

HRID 1403375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-chloro-2,3-dihydro-1-benzofuran-3-one (2.5 g, 14.83 mmol) in methanol (50 mL) was treated with NaBH4 (1.2 g, 31.58 mmol) in four equivalent portions at room temperature, until the reaction was complete, as monitored by TLC (1 h). The reaction mixture was quenched by the addition of acetone (10 mL). This mixture was then treated with HCl (3N, 20 mL). After stirring for another 1 h, the resulting solution was extracted with ethyl acetate (3×50 mL) dried over anhydrous magnesium sulfate and concentrated under vacuum to give 6-chloro-1-benzofuran as oil (2 g, crude).

WORKUP

后处理

  1. customas monitored by TLC (1 h)
  2. customThe reaction mixture was quenched by the addition of acetone (10 mL)
  3. additionThis mixture was then treated with HCl (3N, 20 mL)
  4. extractionthe resulting solution was extracted with ethyl acetate (3×50 mL)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under vacuum