HRID1870866

反应详情

EQUATION

反应方程式

HRID 1870866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared from 3-(4-chlorophenyl)-8-methyl-8-azabicyclo[3.2.1]octan-3-ol (4 g, 16 mmol), glacial acetic acid (15 mL) and concentrated hydrochloric acid (15 mL). Yield of free base (3.6 g, 97%). Some of the free base (1.44 g, 6 mmol) was dissolved in ethanol (96%) and added malonic acid (0.62 g, 6 mmol) in ethanol (96%). The resulting solution was concentrated to an oil, the oil was trituated in diethyl ether, the title compound precipitated as powder and was isolated by filtration. Yield (1.4 g, 71%) as white crystals m.p. 100.8-102.1° C.

WORKUP

后处理

  1. concentrationThe resulting solution was concentrated to an oil
  2. customthe title compound precipitated as powder
  3. customwas isolated by filtration