HRID2418284

反应详情

EQUATION

反应方程式

HRID 2418284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9-(4-Methylbenzyl)-9-aza-bicyclo-[3.3.1]-nonan-3-one oxime (4 g) was dissolved in amyl alcohol (100 ml) and heated to reflux. Sodium (2 g) was added portionwise whilst the solution was stirred. After all the sodium had dissolved, the solution was cooled, diluted with ether and acidified with dilute hydrochloric acid. The acid extract was washed with ether and then basified with excess potassium carbonate. Extraction with ethyl acetate followed by evaporation of solvent afforded crude 3-amino-9-(4-methylbenzyl)-9-azabicyclo[3.3.1]-nonane (3.6 g, 95%) used in the next procedure without purification.

WORKUP

后处理

  1. temperatureheated to reflux
  2. temperaturethe solution was cooled
  3. extractionThe acid extract
  4. washwas washed with ether
  5. extractionExtraction with ethyl acetate
  6. customfollowed by evaporation of solvent