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Ethyl Acetate → HCID 58577251、化合物

HRID 82687
ノート
印刷プレビュー

反応式

HRID 82687 の反応式
C([O:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:19]3=[N:20][CH:21]=[CH:22][C:23]([CH3:24])=[C:18]3[N:17]([CH3:25])[C:16]2=[O:26])=[CH:11][CH:10]=1)C1C=CC=CC=1.CCOC(C)=O>CN(C=O)C.[Pd]>[OH:8][C:9]1[CH:10]=[CH:11][C:12]([N:15]2[C:19]3=[N:20][CH:21]=[CH:22][C:23]([CH3:24])=[C:18]3[N:17]([CH3:25])[C:16]2=[O:26])=[CH:13][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 585774663-[4-(benzyloxy)phenyl]-1,7-dimethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

生成物 1

HCID 58577251HCID 58577251、化合物収率 87.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3-[4-(benzyloxy)phenyl]-1,7-dimethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (2.0 g) and 10% Pd—C (0.308 g) in DMF (10 mL)-EtOAc (100 mL) was hydrogenated under balloon pressure at 20° C. for 1 h. The catalyst was removed by filtration and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (NH silica gel, eluted with 50%-100% EtOAc in hexane) to give 3-(4-hydroxyphenyl)-1,7-dimethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (1.30 g) as a light brown solid. This product was subjected to the next reaction without further purification.

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was purified by column chromatography (NH silica gel, eluted with 50%-100% EtOAc in hexane)

出典と根拠

ORDレコード
ord-fd0607150dfe42f3b30b08a7574d076e
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846713B2

反応ノート

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