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Methanol → 1-[({2,5-Difluoro-4-[(2-{[(3-hydroxyazetidin-1-yl)carbonyl]amino}pyridin-4-yl)oxy]phenyl}amino)carbonyl]cyclopropanecarboxylic acid triethylamine salt

HRID 388522
ノート
印刷プレビュー

反応式

HRID 388522 の反応式
[F:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:21][CH:20]([OH:22])[CH2:19]3)=[O:17])[CH:10]=2)[C:5]([F:23])=[CH:4][C:3]=1[NH:24][C:25]([C:27]1([C:30]([O:32]CC2C=CC=CC=2)=[O:31])[CH2:29][CH2:28]1)=[O:26].CO.[H][H].[CH2:44]([N:46]([CH2:49][CH3:50])[CH2:47][CH3:48])[CH3:45]>O1CCCC1.[Pd]>[CH2:44]([N:46]([CH2:49][CH3:50])[CH2:47][CH3:48])[CH3:45].[F:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:19][CH:20]([OH:22])[CH2:21]3)=[O:17])[CH:10]=2)[C:5]([F:23])=[CH:4][C:3]=1[NH:24][C:25]([C:27]1([C:30]([OH:32])=[O:31])[CH2:29][CH2:28]1)=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 8471TriethylamineHCID 24788565Benzyl 1-[({2,5-difluoro-4-[(2-{[(3-hydroxyazetidin-1-yl)carbonyl]amino}pyridin-4-yl)oxy]phenyl}amino)carbonyl]cyclopropanecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 247885641-[({2,5-Difluoro-4-[(2-{[(3-hydroxyazetidin-1-yl)carbonyl]amino}pyridin-4-yl)oxy]phenyl}amino)carbonyl]cyclopropanecarboxylic acid triethylamine salt
収率 88%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

Benzyl 1-[({2,5-difluoro-4-[(2-{[(3-hydroxyazetidin-1-yl)carbonyl]amino}pyridin-4-yl)oxy]phenyl}amino)carbonyl]cyclopropanecarboxylate (84.2 mg) was dissolved in tetrahydrofuran and methanol (1:1) (2 ml) under a nitrogen atmosphere. 10% palladium on carbon (33.2 mg) was added and the air in the reaction vessel was replaced by hydrogen, and the mixture was stirred at room temperature for 20 hours. The air in the reaction vessel was replaced by nitrogen, and triethylamine (0.0435 ml) was added, and the mixture was stirred for 30 minutes. The catalyst was removed by filtration, and washed with methanol. The filtrate was concentrated under reduced pressure to give the title compound (75.3 mg, 88%) as a white solid.

後処理

  1. additionwas added
  2. stirringthe mixture was stirred for 30 minutes
  3. customThe catalyst was removed by filtration
  4. washwashed with methanol
  5. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b2701c40d7c0484b9c23790b2b55e827
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08377938B2

反応ノート

読み込み中…

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