HRID501845

反应详情

EQUATION

反应方程式

HRID 501845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(4—Nitrophenoxy)-acetic acid-2-[2-(4-nitrophenoxy)-acetoxy]-ethyl ester 24 (100 g, 238 mmol) was dissolved in dry dimethyl formamide (500 ml) in a pressure vessel, palladium on carbon (5%, 22 g) was added, and the mixture stirred under an atomsphere of hydrogen (4 kg) for 6 hours. The catalyst was removed by filtration and ice water (2.5 L) was added to the filtrate. Crude 25 was filtered off, dried and recrystallised in a mixture of methanol:chloroform (1:1) to give pure 25 (65 g, 78%) as a light brown shining powder with an m.p. between 124-125.8° C.

WORKUP

后处理

  1. customThe catalyst was removed by filtration and ice water (2.5 L)
  2. additionwas added to the filtrate
  3. filtrationCrude 25 was filtered off
  4. customdried
  5. customrecrystallised in a mixture of methanol:chloroform (1:1)