HRID1196233

反应详情

EQUATION

反应方程式

HRID 1196233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

(3aRS,7aRS)-7,7-Diphenyl-2-vinyloxycarbonylperhydro-4-isoindolone (177 g) is treated with a 5.7N solution (1000 cc) of hydrochloric acid in dry dioxane for 30 minutes at 20° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the residue taken up in ethanol (500 cc), and the reaction mixture is stirred at 60° C. for 30 minutes and then cooled to +5° C. The crystals obtained are drained, washed with ethanol (50 cc) and dried. (3aRS,7aRS)-7,7-Diphenylperhydro-4-isoindolone hydrochloride (130 g), m.p. 270° C. with decomposition, is obtained.

WORKUP

后处理

  1. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  2. temperaturecooled to +5° C
  3. customThe crystals obtained
  4. washwashed with ethanol (50 cc)
  5. customdried