HRID26526

反应详情

EQUATION

反应方程式

HRID 26526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.262 g of 3-bromo-11H-s-triazolo [3,4-b][3]benzazepine in 2 ml of methanol was added 1.0 ml of 2 N-sodium methoxide/methanol and the mixture was refluxed for one hour. The solvent was evaporated off and, following the addition of water, the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with isopropyl ether. By the above procedure was obtained 3-methoxy-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethyl acetate-n-hexane yielded colorless prisms, melting point: 161°-162° C. The infrared absorption spectrum of this product was identical with that of the compound obtained in Example 34.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for one hour
  2. customThe solvent was evaporated off
  3. additionthe addition of water
  4. extractionthe residue was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over Na2SO4
  7. customThe solvent was then evaporated off
  8. additionthe residue was treated with isopropyl ether