HRID1589705

反应详情

EQUATION

反应方程式

HRID 1589705 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrogen gas was passed for 2 hours through a mixture of 3.6 g of 6-acetoxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman-4-one, 1 g of 10% w/w palladium-on-carbon and 100 ml of methanol at room temperature under atmospheric pressure. The catalyst was then removed by filtration and the filtrate was condensed by evaporation under reduced pressure. The residue was subjected to silica gel column chromatography, eluted with a 2:1 by volume mixture of hexane and ethyl acetate, and the resulting crude product was recrystallized from acetone, to yield 6-acetoxy-2-(4-aminophenoxymethyl)-2,5,7,8-tetramethylchroman-4-one. Its melting point was 177°-178° C.

WORKUP

后处理

  1. customThe catalyst was then removed by filtration
  2. customcondensed
  3. customby evaporation under reduced pressure
  4. washeluted with a 2:1 by volume mixture of hexane and ethyl acetate
  5. customthe resulting crude product was recrystallized from acetone