HRID2120959

反应详情

EQUATION

反应方程式

HRID 2120959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

11.65 g (50 mmol) N-(benzyloxycarbonyl)piperidone (prepared from 4-piperidone and benzyl chloroformate according to Chem. Pharm. Bull. 1982, 30, 1084) and 7.2 g (50 mmol) benzylamine hydrochloride were dissolved in a mixture of 20 ml methanol and 10 ml water. The solution was kept at 0° C., while 15 ml of an aqueous solution of 3.26 g (50 mmol) potassium cyanide were added dropwise. After stirring overnight at room temperature a crystalline solid had been formed, which was collected by filtration. The filtrate was treated with a mixture of water and ether. The organic layer was separated and the aqueous layer extracted with ether. The combined organic layers were dried over sodium sulfate and added to the solid material. The title hydrochloride precipitated after treating with a saturated ethereal solution of hydrogen chloride, and it was isolated by filtration and dried in vacuo.

WORKUP

后处理

  1. additionwere added dropwise
  2. customhad been formed
  3. filtrationwhich was collected by filtration
  4. additionThe filtrate was treated with a mixture of water and ether
  5. customThe organic layer was separated
  6. extractionthe aqueous layer extracted with ether
  7. dry with materialThe combined organic layers were dried over sodium sulfate
  8. additionadded to the solid material
  9. customThe title hydrochloride precipitated
  10. additionafter treating with a saturated ethereal solution of hydrogen chloride
  11. customit was isolated by filtration
  12. customdried in vacuo