تفاعل #2045053
ord-9b92a38367da4e5dae4008eaed0cc8ab
معادلة التفاعل
4-(6-Benzyloxyhexanoylamino)phenoxyacetic acid methyl ester
→
77
المردود 24.4%
4-(6-Hydroxyhexanoylamino)phenoxyacetic acid methyl ester
المردود 24.4%
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىCatalyst was removed by filtration
- 2workup.DISTILLATIONthe solvents were distilled off under vacuum
- 3أخرىCrude 77 was purified by column chromatography on silica gel
الإجراء التجريبي
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.