HRID1386563

反应详情

EQUATION

反应方程式

HRID 1386563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.46 g of (E)-2(R)-[1(S)-[(tetrahydro-2(RS)-pyranyloxy)carbamoyl]-4-phenyl-3-butenyl]-2′-isobutyl-2′-(1,3-dioxo-2-phthalimidoethansulphonyl)-4-methylvalerohydrazide in 10 ml of ethanol was treated with 4.5 ml of hydrazine hydrate and stirred at room temperature for 2 hours. Evaporation gave a residue which was triturated with ethyl acetate and filtered. The filtrate was washed with water and saturated aqueous sodium chloride and then dried over anhydrous magnesium sulphate. The residue was purified by column chromatography on silica gel using methanol/dichloromethane (5:95) for the elution to give 0.26 g of (E)-2′-(2-aminoethanesulphonyl)-2(R)-[1(S)-[(tetrahydro-2(RS)-pyranyloxy)carbamoyl]-4-phenyl-3-butenyl]-2′-isobutyl-4-methylvalerohydrazide in the form of a pale yellow gum.

WORKUP

后处理

  1. customEvaporation
  2. customgave a residue which
  3. customwas triturated with ethyl acetate
  4. filtrationfiltered
  5. washThe filtrate was washed with water and saturated aqueous sodium chloride
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customThe residue was purified by column chromatography on silica gel
  8. washfor the elution