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Methylamine → 1,1-Dimethylethyl 7-({5-[(methylamino)carbonyl]-2-pyrazinyl}oxy)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

HRID 645797
ノート
印刷プレビュー

反応式

HRID 645797 の反応式
[C:1](N1C=CN=C1)([N:3]1C=CN=C1)=O.[CH3:13][C:14]([O:17][C:18]([N:20]1[CH2:26][CH2:25][C:24]2[CH:27]=[CH:28][C:29]([O:31][C:32]3[N:33]=[CH:34][C:35]([C:38]([OH:40])=O)=[N:36][CH:37]=3)=[CH:30][C:23]=2[CH2:22][CH2:21]1)=[O:19])([CH3:16])[CH3:15].CN>ClCCl>[CH3:1][NH:3][C:38]([C:35]1[N:36]=[CH:37][C:32]([O:31][C:29]2[CH:28]=[CH:27][C:24]3[CH2:25][CH2:26][N:20]([C:18]([O:17][C:14]([CH3:13])([CH3:16])[CH3:15])=[O:19])[CH2:21][CH2:22][C:23]=3[CH:30]=2)=[N:33][CH:34]=1)=[O:40]
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 3

HCID 6329MethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 574376215-[(3-{[(1,1-Dimethylethyl)oxy]carbonyl}-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-2-pyrazinecarboxylic acid

生成物 1

HCID 685073281,1-Dimethylethyl 7-({5-[(methylamino)carbonyl]-2-pyrazinyl}oxy)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate収率 66.8%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

1,1′-Carbonyldiimidazole (16.6 g, 102 mmol) was added to a solution of 5-[(3-{[(1,1-dimethylethyl)oxy]carbonyl}-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-2-pyrazinecarboxylic acid (D49, Step 2) (37.5 g, 97 mmol) in dry dichloromethane (400 ml) and the resulting mixture was stirred at room temperature for 18 hours. Methylamine (2M solution in tetrahydrofuran) (100 ml) was added and the mixture stirred for 2 hours. The solvent was removed in vacuo and the residue was purified by column chromatography eluting with a mixture of ethyl acetate:chloroform (1:1) to afford the title compound (25.8 g); MS (ES+) m/e 399 [M+H]+.

後処理

  1. stirringthe mixture stirred for 2 hours
  2. customThe solvent was removed in vacuo
  3. customthe residue was purified by column chromatography
  4. washeluting with a mixture of ethyl acetate:chloroform (1:1)

出典と根拠

ORDレコード
ord-aebf0d90299c486ab8c9eafd4c6bc262
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07704994B2

反応ノート

読み込み中…

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