反応 #2045054

ord-6cd49050e6f4430f83d6887c11fd25e2

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Catalyst was removed by filtration and methanol
  2. 2
    workup.DISTILLATIONdistilled off
  3. 3
    その他The crude 79 was purified by column chromatography on silica gel

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08409559B2uspto-grants-2013_04