HRID443799

反应详情

EQUATION

反应方程式

HRID 443799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The starting material is obtained as follows. The solution of 13.35 g of 4-diphenylmethoxypiperidine in 40 ml of methanol, containing 3.52 g of ethylene oxide and 0.9 ml of water, is stirred and heated in an oil bath at 42°-44° for 4 hours. The bath temperature is raised to 50° and heating and stirring are continued for an additional 3 hours. The solution is then evaporated and the residue taken up in 1 N hydrochloric acid and washed with diethyl ether. The aqueous solution is made basic with 50% aqueous sodium hydroxide and repeatedly extracted with diethyl ether. The extract is washed with brine, dried and evaporated to give the 1-(2-hydroxyethyl)-4-diphenylmethoxypiperidine, melting at 83°-85° after recrystallization from cyclohexane.

WORKUP

后处理

  1. customThe starting material is obtained
  2. temperatureheated in an oil bath at 42°-44° for 4 hours
  3. temperatureThe bath temperature is raised to 50°
  4. temperatureheating
  5. stirringstirring
  6. customThe solution is then evaporated
  7. washwashed with diethyl ether
  8. extractionrepeatedly extracted with diethyl ether
  9. washThe extract is washed with brine
  10. customdried
  11. customevaporated