HRID638732
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe catalyst was removed by filtration and ice water (2.5 L)
- additionwas added to the filtrate
- filtrationCrude 43 was filtered off
- customdried
- customrecrystallised in a mixture of methanol:chloroform (1:1)