反应详情

2-(4-nitrophenoxy)propionic acid-2-[2-(4-nitrophenoxy)propionyloxy]ethyl ester 49 (50 g, 89.3 mmol) was dissolved in dry dimethylformamide (400 ml) in a pressure vessel, palladium on carbon (5%, 12.5 g) added, and the mixture stirred under an atm. of hydrogen (4 Kg) for 4 hours. The catalyst was removed by filtration and ice water (3 L) was added to the filtrate. Crude 50 was extracted into ethyl acetate, dried over Na2SO4, distilled and purified by column chromatography on silica gel using chloroform as eluant to give pure 50 (25 g, 58%) as a syrup.

1. customThe catalyst was removed by filtration and ice water (3 L)
2. additionwas added to the filtrate
3. extractionCrude 50 was extracted into ethyl acetate
4. dry with materialdried over Na2SO4
5. distillationdistilled
6. custompurified by column chromatography on silica gel