HRID261474

反应详情

EQUATION

反应方程式

HRID 261474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3 ml of acetyl chloride in 10 ml of chloroform is added dropwise to a stirred suspension of 6.0 g of 2,3-dihydrospiro[benzofuran-2,4'-piperidine], Example 1C, and 14.0 g of sodium bicarbonate in 75 ml of chloroform. After total addition, the reaction mixture is successively stirred at ambient temperature for 16 hours, filtered, washed sequentially with water, dilute hydrochloric acid and a saturated sodium chloride solution, dried and the solvent removed under reduced pressure, leaving a residue which solidifies upon standing. The solid is recrystallized twice from hexane to give the product, 2,3-dihydro-1'-acetylspiro[benzofuran-2,4'-piperidine], mp 94°-97° C.

WORKUP

后处理

  1. additionAfter total addition
  2. filtrationfiltered
  3. washwashed sequentially with water, dilute hydrochloric acid
  4. dry with materiala saturated sodium chloride solution, dried
  5. customthe solvent removed under reduced pressure
  6. customleaving a residue which
  7. customThe solid is recrystallized twice from hexane