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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 222664
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HRID 222664 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

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]+.

후처리

  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)

출처 및 근거

ORD 기록
ord-79f142cc95794a78b59fb87181da67bd
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08207331B2

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