Methanol → N-{3-[(5-aminopyridin-2-yl)oxy]-4-methoxyphenyl}-3-(1-cyanocyclopropyl)benzamide

HRID 1800423ノート

反応式

HRID 1800423 の反応式
[C:1]([C:3]1([C:6]2[CH:7]=[C:8]([CH:30]=[CH:31][CH:32]=2)[C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[C:14]([O:20][C:21]3[CH:26]=[CH:25][C:24]([N+:27]([O-])=O)=[CH:23][N:22]=3)[CH:13]=2)=[O:10])[CH2:5][CH2:4]1)#[N:2].CO>O1CCCC1.[C].[Pd]>[NH2:27][C:24]1[CH:25]=[CH:26][C:21]([O:20][C:14]2[CH:13]=[C:12]([NH:11][C:9](=[O:10])[C:8]3[CH:30]=[CH:31][CH:32]=[C:6]([C:3]4([C:1]#[N:2])[CH2:5][CH2:4]4)[CH:7]=3)[CH:17]=[CH:16][C:15]=2[O:18][CH3:19])=[N:22][CH:23]=1

参加物

5

反応物 2

HCID 887MethanolHCID 684192063-(1-cyanocyclopropyl)-N-{4-methoxy-3-[(5-nitropyridin-2-yl)oxy]phenyl}benzamide

生成物 1

HCID 68418573N-{3-[(5-aminopyridin-2-yl)oxy]-4-methoxyphenyl}-3-(1-cyanocyclopropyl)benzamide収率 102.5%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-(1-cyanocyclopropyl)-N-{4-methoxy-3-[(5-nitropyridin-2-yl)oxy]phenyl}benzamide (4.30 g, 9.99 mmol) in tetrahydrofuran (100 mL) were added methanol (50 mL) and 10% palladium-carbon (982 mg), and the mixture was stirred at room temperature for 14 hr under a hydrogen atmosphere (2.5 atm). The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (4.1 g) as a brown syrup substance. The syrup substance was used for the next reaction without further purification.

後処理

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-5196e962a4c84675aec31fd9f01900cf
出典データセット
uspto-grants-2013_01
特許番号
US08344135B2

反応ノート

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