HRID1643435

反应详情

EQUATION

反应方程式

HRID 1643435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrogen chloride in methanol (1.25 mol/l, 6.3 ml) was added to tert-butyl 9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carboxylate (0.52 g, 1.569 mmol) and the mixture was refluxed for 1 h. The solvent was removed in vacuo, the residue taken up in ethanol (3 ml) and the mixture cooled. Acetone (80 ml) was added and the mixture was stirred in an ice bath for 30 min. The precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. temperaturethe mixture cooled
  4. additionAcetone (80 ml) was added
  5. filtrationThe precipitate was filtered out with suction
  6. washwashed with diethyl ether
  7. customdried in vacuo