HRID1253676

反应详情

EQUATION

反应方程式

HRID 1253676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Hydrogen chloride in methanol (1.25 mol/l, 15.9 ml) was added to tert-butyl 2-(pyridin-4-yl)-2,9-diazaspiro[5.5]undecane-9-carboxylate (0.66 g, 1.991 mmol) and the mixture was refluxed for 2 h. The solvent was removed in vacuo, the residue was taken up in ethanol (5 ml) and the mixture was cooled. Acetone (20 ml) was added and the mixture was stirred at 0° C. for 30 min. Diethyl ether (50 ml) was added and the precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo. Yield: 0.42 g (69%)

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 h
  2. customThe solvent was removed in vacuo
  3. temperaturethe mixture was cooled
  4. additionAcetone (20 ml) was added
  5. additionDiethyl ether (50 ml) was added
  6. filtrationthe precipitate was filtered out with suction
  7. washwashed with diethyl ether
  8. customdried in vacuo