反応 #2045053

反応方程式

4-(6-Benzyloxyhexanoylamino)phenoxyacetic acid methyl ester

→

77

収率 24.4%

4-(6-Hydroxyhexanoylamino)phenoxyacetic acid methyl ester

収率 24.4%

溶媒

methanol

dimethylformamide

反応条件

後処理

1. 1
   その他Catalyst was removed by filtration
2. 2
   workup.DISTILLATIONthe solvents were distilled off under vacuum
3. 3
   その他Crude 77 was purified by column chromatography on silica gel

実験手順

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.

出典