HRID1460646

反应详情

EQUATION

反应方程式

HRID 1460646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A sample of the above alcohol (140 g, 0.70 mole) was dissolved in toluene (400 ml) and thionyl bromide (80 ml, 0.77 mole) was introduced with vigorous stirring. After 1.5 h the exotherm reaction had subsided and diethyl ether (400 ml) was added. The resultant precipitate was collected by filtration and washed with diethyl ether. The solid was triturated with ethyl acetate, again collected on a filter and dried to provide (R)-1-(2-bromoethyl)nipecotic acid ethyl ester hydrobromide (175 g, 73%) as a white solid, m.p. 210°-215° C.

WORKUP

后处理

  1. customAfter 1.5 h the exotherm reaction
  2. filtrationThe resultant precipitate was collected by filtration
  3. washwashed with diethyl ether
  4. customThe solid was triturated with ethyl acetate
  5. customagain collected on
  6. filtrationa filter
  7. customdried