반응 #2045054

ord-6cd49050e6f4430f83d6887c11fd25e2

반응 방정식

COC(=O)C(C)Oc1ccc(NC(=O)CCCCCOCc2ccccc2)cc1
2-[4-(6-Benzyloxyhexanoylamino)phenoxy]propionic acid methyl ester
COC(=O)C(C)Oc1ccc(NC(=O)CCCCCO)cc1
79
수율 51.6%
COC(=O)C(C)Oc1ccc(NC(=O)CCCCCO)cc1
2-[4-(6-Hydroxyhexanoylamino)phenoxy]propionic acid methyl ester
수율 51.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Catalyst was removed by filtration and methanol
  2. 2
    workup.DISTILLATIONdistilled off
  3. 3
    기타The crude 79 was purified by column chromatography on silica gel

실험 절차

2-[4-(6-Benzyloxyhexanoylamino)phenoxy]propionic acid methyl ester 78 (15 g, 37.59 mmol) was dissolved in methanol (150 ml) in a pressure vessel, palladium on carbon (50% wet, 5%, 15 g) added and the mixture stirred under a hydrogen atmosph. (4 Kg) for 16 hrs. Catalyst was removed by filtration and methanol distilled off. The crude 79 was purified by column chromatography on silica gel using chloroform as eluant to get pure 79 (6 g, 51.6%) as a white powder. M.p: 62-64.5° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08409559B2uspto-grants-2013_04