HRID459897

反应详情

EQUATION

反应方程式

HRID 459897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-benzyloxycarbonylamino-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepin-2-one (1.00 g, 2.59 mmol) in dimethylformamide (10 mL) was cooled to 0° C. under argon. Sodium hydride (60 wt %, 156 mg, 3.89 mmol) was added followed by isobutyl iodide. Let warm to room temperature and stirred overnight. The reaction was worked up with methylene chloride and saturated sodium chloride. The organic extracts were dried over sodium sulfate, filtered and concentrated. Chromatography (silica gel, 5 to 50% ethyl acetate in hexane gradient elution), giving the title compound (0.92 g). MS 442 (M+1).

WORKUP

后处理

  1. dry with materialThe organic extracts were dried over sodium sulfate
  2. filtrationfiltered
  3. concentrationconcentrated
  4. washChromatography (silica gel, 5 to 50% ethyl acetate in hexane gradient elution)