HRID1075025

反应详情

EQUATION

反应方程式

HRID 1075025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add to 25 cc. of tetrahydrofuran cooled in an ice bath 1.59 gm. (11.9 mmole) of aluminum chloride, 1.33 gm. (5.25 mmole) of 3-cyanomethyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin and 1.55 gm. (23.8 mmole) of sodium azide. Reflux the mixture for 19 hours, cool, dilute with water and acidify. Extract the mixture into ethyl acetate and evaporate. Triturate the residue in ether and separate the title product by filtration.

WORKUP

后处理

  1. additionAdd to 25 cc
  2. temperatureReflux the mixture for 19 hours
  3. temperaturecool
  4. extractionExtract the mixture into ethyl acetate
  5. customevaporate
  6. customTriturate the residue in ether
  7. customseparate the title product
  8. filtrationby filtration