HRID2073381

反应详情

EQUATION

反应方程式

HRID 2073381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8-bromomethyl-1,1-dimethyl-2(1H)-naphtho[2,1-b]furanone in acetonitrile (5 ml), was treated with 1,2,4-triazole (1.4 g) and the mixture was heated under reflux for 18 h. The solution was evaporated to dryness under reduced pressure and the residue was partitioned between 1N aqueous sodium hydrogen carbonate and ethyl acetate. The ethyl acetate extract was separated, dried and evaporated to dryness, and the residue was purified by flash chromatography. Elution with methanol:chloroform, 1:49 v/v, gave 1,1-dimethyl-8-(1H-1,2,4-triazol-1-ylmethyl)-2-(1H)-naphtho[2,1-b]furanone, m.p. 136°-137° after recrystallisation from a mixture of ethyl acetate and cyclohexane.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 18 h
  3. customThe solution was evaporated to dryness under reduced pressure
  4. customthe residue was partitioned between 1N aqueous sodium hydrogen carbonate and ethyl acetate
  5. extractionThe ethyl acetate extract
  6. customwas separated
  7. customdried
  8. customevaporated to dryness
  9. customthe residue was purified by flash chromatography
  10. washElution with methanol