HRID1632779

反应详情

EQUATION

反应方程式

HRID 1632779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The 3-amino-5-methyl-1,3,4,5-tetrahydro-1,5-benzodiazepin-2-one (0.267 g) is dissolved in 5 ml of methanol and 0.288 g of ethyl 2-oxo-4-phenylbutyrate is added. This is followed by the addition of a solution of 88 mg of sodium cyanoborohydride in 3 ml of methanol and 0.8 ml of glacial acetic acid. The reaction is stirred overnight under nitrogen and concentrated. The residue is dissolved in 20 ml of methylene chloride and washed with 10 ml of cold saturated sodium carbonate. After drying over magnesium sulfate the solution is concentrated and the residue purified to give 3-[N-(1-carboethoxy-3-phenylpropyl)amino]-5-methyl-1,3,4,5-tetrahydro-1,5-benzodiazepin-2(2H)-one.

WORKUP

后处理

  1. concentrationconcentrated
  2. dissolutionThe residue is dissolved in 20 ml of methylene chloride
  3. washwashed with 10 ml of cold saturated sodium carbonate
  4. dry with materialAfter drying over magnesium sulfate the solution
  5. concentrationis concentrated
  6. customthe residue purified