HRID1049776

反应详情

EQUATION

反应方程式

HRID 1049776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-[4-[3-(Methylthio)benzoylamino]phenyl]-1H-naphtho[1,2-b][1,4]diazepine-2,4(3H,5H)-dione (20 mg, 0.043 mmol) obtained in Example 126 was dissolved in dimethylformamide (0.4 mL), the solution was added with m-chloroperbenzoic acid (ii mg, 0.03 mmol) at −20° C., and the mixture was stirred for 30 minutes. After completion of the reaction, the reaction mixture was added with ethyl acetate at −20° C., the organic layer was washed with saturated aqueous sodium hydrogencarbonate, water, and saturated brine. The solvent of the organic layer was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (chloroform/methanol=100/1) to obtain the title compound (8 mg, yield 38%).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. washthe organic layer was washed with saturated aqueous sodium hydrogencarbonate, water, and saturated brine
  3. customThe solvent of the organic layer was evaporated under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography (chloroform/methanol=100/1)