HRID1651476

反应详情

EQUATION

反应方程式

HRID 1651476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ammonium formate (8.0 g) was added to a stirred and cooled mixture of 5-t-butyl-2-methoxy-3-nitrophenyl N-t-butyl-sulfonamide (8.0 g) and 10% Palladium on charcoal (1.1 g) in dry methanol (80 ml) under nitrogen. The mixture was stirred at ambient temperature for 1 hour and then filtered through diatomaceous earth. The filtrate was concentrated and taken up into a mixture of ethyl acetate and water. The organic layer was separated and dried over sodium sulphate. After removal of solvent and recrystallization from aqueous ethanol the title compound was obtained as white crystals (6.9 g).

WORKUP

后处理

  1. temperaturecooled
  2. stirringThe mixture was stirred at ambient temperature for 1 hour
  3. filtrationfiltered through diatomaceous earth
  4. concentrationThe filtrate was concentrated
  5. additiontaken up into a mixture of ethyl acetate and water
  6. customThe organic layer was separated
  7. dry with materialdried over sodium sulphate
  8. customAfter removal of solvent and recrystallization from aqueous ethanol the title compound