反应详情

(4-Nitrophenoxy)-acetic acid methoxycarbonyl methyl ester 44 (20 g, 74.3 mmol) was dissolved in dimethyl formamide (100 ml) in a pressure vessel. Palladium on carbon (5%, 8 g) was added, and the mixture stirred under an atmosphere of hydrogen (4 kg) for 2 hours. The catalyst was removed by filtration and ice water (400 ml) was added to the filtrate. Crude 45 was extracted into ethyl acetate, dried over Na2SO4 and distilled. Crude 45 was then recrystallised from chloroform:hexane (1:6) to get pure 45 (13 g, 73%) as a light brown shining powder with an m.p. between 76.5-78.5° C.

1. customThe catalyst was removed by filtration and ice water (400 ml)
2. additionwas added to the filtrate
3. extractionCrude 45 was extracted into ethyl acetate
4. dry with materialdried over Na2SO4
5. distillationdistilled
6. customCrude 45 was then recrystallised from chloroform:hexane (1:6)