반응 #2045053

반응 방정식

4-(6-Benzyloxyhexanoylamino)phenoxyacetic acid methyl ester

→

77

수율 24.4%

4-(6-Hydroxyhexanoylamino)phenoxyacetic acid methyl ester

수율 24.4%

용매

methanol

dimethylformamide

반응 조건

후처리

1. 1
   기타Catalyst was removed by filtration
2. 2
   workup.DISTILLATIONthe solvents were distilled off under vacuum
3. 3
   기타Crude 77 was purified by column chromatography on silica gel

실험 절차

4-(6-Benzyloxyhexanoylamino)phenoxyacetic acid methyl ester 76 (24 grams, 62.33 mmol) was dissolved in a mixture of methanol (200 ml) and dimethylformamide (50 ml) in a pressure vessel, palladium on carbon (5%, 15 g) was added and the mixture stirred under a hydrogen atm. (4 Kg) for 24 hrs. Catalyst was removed by filtration, and the solvents were distilled off under vacuum. Crude 77 was purified by column chromatography on silica gel using chloroform as eluant to get pure 77 (4.5 g, 24.4%) as a white powder. M.p: 87.5-90.4° C.

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