HRID2296066

反应详情

EQUATION

反应方程式

HRID 2296066 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An amount of 7.0 g of 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-methanol is dissolved in 50 ml of absolute pyridine; to the solution are added 2.4 ml of acetic anhydride, and the whole is then allowed to stand for 17 hours at 25°. The reaction mixture is afterwards concentrated in vacuo. The residue is dissolved in methylene chloride, and the solution washed with water and saturated sodium chloride solution, dried over sodium sulphate, and concentrated by evaporation. After crystallisation of the residue from ethyl/acetate is obtained 1-(acetoxymethyl)-6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine, M.P. 210°-212°.

WORKUP

后处理

  1. concentrationThe reaction mixture is afterwards concentrated in vacuo
  2. dissolutionThe residue is dissolved in methylene chloride
  3. washthe solution washed with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation
  6. customAfter crystallisation of the residue from ethyl/acetate