HRID270047

反应详情

EQUATION

反应方程式

HRID 270047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1′-benzyl-6-chloro-3,4-dihydrospiro[chromene-2,4′-piperidine] (1.63 g, 5.0 mmol) and 1-chloroethyl chloroformate (1.07 g, 7.5 mmol) in toluene (5 ml) was heated with reflux overnight. The solvent was removed i. vacuo, the oily residue dissolved in methanol (10 ml) and heated with reflux overnight. The solvent was removed in vacuo, and the residue treated with diethyl ether (50 ml). The white precipitate was collected by filtration, washed with diethyl ether and dried to afford the subtitle compound as white powder (0.58 g, 49%).

WORKUP

后处理

  1. temperaturewith reflux overnight
  2. customThe solvent was removed i
  3. dissolutionvacuo, the oily residue dissolved in methanol (10 ml)
  4. temperatureheated
  5. temperaturewith reflux overnight
  6. customThe solvent was removed in vacuo
  7. additionthe residue treated with diethyl ether (50 ml)
  8. filtrationThe white precipitate was collected by filtration
  9. washwashed with diethyl ether
  10. customdried