4-(2-Benzyloxyacetylamino)phenoxyacetic acid methyl ester → 4-(2-Hydroxyacetylamino)phenoxyacetic acid methyl ester

HRID 2169743ノート

反応式

HRID 2169743 の反応式
[CH3:1][O:2][C:3](=[O:24])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:23])[CH2:14][O:15]CC2C=CC=CC=2)=[CH:8][CH:7]=1>CO.[Pd]>[CH3:1][O:2][C:3](=[O:24])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:23])[CH2:14][OH:15])=[CH:8][CH:7]=1

参加物

4

反応物 1

HCID 592539834-(2-Benzyloxyacetylamino)phenoxyacetic acid methyl ester

生成物 1

HCID 592539714-(2-Hydroxyacetylamino)phenoxyacetic acid methyl ester収率 77%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

4-(2-Benzyloxyacetylamino)-phenoxyacetic acid methyl ester 66 (25 g, 76 mmol) was dissolved in methanol (450 ml) in a pressure vessel, palladium on carbon (5%, 10 g) added and the mixture stirred under a hydrogen atm. (2 Kg) for 5 hrs. Catalyst was removed by filtration and methanol distilled off. Crude 67 was recrystallised in chloroform:hexane (1:6) to give pure 67 (14 g) as a white powder. M.p: 147.5-150° C.

後処理

  1. customCatalyst was removed by filtration and methanol
  2. distillationdistilled off
  3. customCrude 67 was recrystallised in chloroform:hexane (1:6)

出典と根拠

ORDレコード
ord-077cb91b742946f3b8b93d99e4db3575
出典データセット
uspto-grants-2015_06
特許番号
USRE045548E1

反応ノート

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