HRID27625

反应详情

EQUATION

反应方程式

HRID 27625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 5.0 g. portion of 8-Chloro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine (Example 1) is added to 2.5 g. of lithium aluminum hydride in 200 ml. of ether. The mixture is stirred and heated under reflux for 4 hours. Water is added dropwise to decompose the excess lithium aluminum hydride. The ether is decanted and the residue is extracted with methylene chloride which is then combined with the ether, dried and evaporated. The residue is crystallized from acetone-hexane giving 8-chloro-10,11-dihydro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine, m.p. 186°-188° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 4 hours
  3. customThe ether is decanted
  4. extractionthe residue is extracted with methylene chloride which
  5. customdried
  6. customevaporated
  7. customThe residue is crystallized from acetone-hexane