HRID2371713

反应详情

EQUATION

反应方程式

HRID 2371713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.70 g of ethyl 4-(dibenz[b,e]oxepin-11(6H)-ylidene)-1-piperidinepropionate, 9.9 ml of 2N sodium hydroxide aqueous solution and 40 ml of methanol was refluxed for 30 min and concentrated. Water was added to the residue, adjusted to pH 3 with 10% hydrochloric acid. The precipitate was collected by filtration and washed with water and ether to give 3.30 g of pale yellow crystals, which were recrystallized from a mixture of water and N,N-dimethylformamide to give 2.75 g of pale yellow crystals, mp 142°-143° C.

WORKUP

后处理

  1. temperaturewas refluxed for 30 min
  2. concentrationconcentrated
  3. additionWater was added to the residue
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water and ether