HRID975869

反应详情

EQUATION

反应方程式

HRID 975869 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 0.070 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one in 2 ml of tetrahydrofuran is added 0.45 ml of a 2.0M solution of diborane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 3 hours, poured into water and made basic with 2N NaOH. The tetrahydrofuran is removed under vacuum and the residual aqueous mixture extracted with diethyl ether. The extract is washed with brine, dried (Na2SO4) and the solvent removed to give 0.065 g of a colorless oil; one spot by thin layer chromatography (silica gel) with ethyl acetate-hexane (1:2) as solvent (Rf 0.81).

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 3 hours
  2. customThe tetrahydrofuran is removed under vacuum
  3. extractionthe residual aqueous mixture extracted with diethyl ether
  4. washThe extract is washed with brine
  5. dry with materialdried (Na2SO4)
  6. customthe solvent removed