HRID638732

反应详情

EQUATION

反应方程式

HRID 638732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(4-nitro-phenoxy)-acetic acid-2-[2-(4-nitrophenoxy) acetoxy]ethyl ester 42 (100 g, 238 mmol) was dissolved in dry dimethylformamide (500 ml) in a pressure vessel, palladium on carbon (5%, 22 g) added, and the mixture stirred under an atmosphere 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 43 was filtered off, dried and recrystallised in a mixture of methanol:chloroform (1:1) to give pure 43 (65 g, 78%) as a light brown shining powder. M.p: 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 43 was filtered off
  4. customdried
  5. customrecrystallised in a mixture of methanol:chloroform (1:1)