HRID726577

反应详情

EQUATION

反应方程式

HRID 726577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of (+) 1-azabicyclo[3.2.1]octan-6-one (124 g, 1 mol) in ethanol (100 ml) was added a solution of (+) camphorsulfonic acid (232 g, 1.0 mol) in 200 ml ethanol. The mixture was heated to 70° C. and slowly cooled over 2 hours to 5° C. The precipitated crystals were collected by filtration and washed with cold ethanol (3×40 ml). The crude compound was crystallized from ethanol (150 ml) giving the title compound in 57.3 g yield. M.p. 267°-268° C. (decomp.). [α]D =+48° (water).

WORKUP

后处理

  1. temperatureslowly cooled over 2 hours to 5° C
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed with cold ethanol (3×40 ml)
  4. customThe crude compound was crystallized from ethanol (150 ml)