HRID596292

反应详情

EQUATION

反应方程式

HRID 596292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice cooled solution of the free base prepared from 1.5 g. of 3',4'-dihydrospiro[cyclohexane-1,2'(1'H)-naphthalen]-4-ylamine hydrochloride [I(c)] (prepared as in Example 10C) in 12 ml. of pyridine, 1 ml. of ethyl chloroformate is added. The mixture is allowed to stand in the cold for about 5 hours and then poured into ice water. The solid that precipitates is collected on a filter and recrystallized from methylene chloride: benzene to give ethyl 3',4'-dihydrospiro[cyclohexane-1,2'(1'H)-naphthalene] -4-carbamate [I(c)].

WORKUP

后处理

  1. customcold for about 5 hours
  2. customThe solid that precipitates
  3. customis collected on
  4. filtrationa filter
  5. customrecrystallized from methylene chloride