HRID1770119

反应详情

EQUATION

反应方程式

HRID 1770119 的结构方程式

PROCEDURE

实验过程

Paraformaldehyde (2.2 g), in 320 ml 2% v/v H2SO4, is heated to boiling and 2.7 g (0.016 mole) of 8-aminomethyl-1,4-dioxaspiro[4,5]decane in 20 ml EtOH, is added over 4 hours. This mixture is then heated at reflux for 24 hours. The cooled reaction is washed with dichloromethane, then basified with 10N NaOH and extracted with dichloromethane. The combined extracts are dried over MgSO4 and stripped to dryness, giving 1.68 g (69%) of product.

WORKUP

后处理

  1. temperatureThis mixture is then heated
  2. temperatureat reflux for 24 hours
  3. customThe cooled reaction
  4. washis washed with dichloromethane
  5. extractionextracted with dichloromethane
  6. dry with materialThe combined extracts are dried over MgSO4