반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[N:8][C:7]([C:15]([NH:17][C:18]1[NH:22][C:21]3[CH:23]=[C:24]([O:30][CH2:31][CH3:32])[CH:25]=[C:26]([C:27]([OH:29])=O)[C:20]=3[N:19]=1)=[O:16])=[CH:6]2.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.S(O)(O)(=O)=O.[NH2:71][C:72]1[NH:73][CH:74]=[CH:75][N:76]=1>CN(C=O)C.[Cl-].[Na+].O>[CH2:31]([O:30][C:24]1[CH:25]=[C:26]([C:27](=[O:29])[NH:71][C:72]2[NH:73][CH:74]=[CH:75][N:76]=2)[C:20]2[NH:19][C:18]([NH:17][C:15]([C:7]3[N:8]=[CH:9][C:10]4[C:5]([CH:6]=3)=[CH:4][C:3]([O:2][CH3:1])=[C:12]([O:13][CH3:14])[CH:11]=4)=[O:16])=[N:22][C:21]=2[CH:23]=1)[CH3:32]참가 물질
7
반응물 4
HCID 81531Diisopropylethylamine
HCID 135136Bis(2-amino-1H-imidazole) sulphate
HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 669408302-[(6,7-dimethoxy-isoquinoline-3-carbonyl)-amino]-6-ethoxy-1H-benzoimidazole-4-carboxylic acid생성물 1
시약·촉매·용매 2
실험 절차
100 mg (0.25 mmol) of 2-[(6,7-dimethoxy-isoquinoline-3-carbonyl)-amino]-6-ethoxy-1H-benzoimidazole-4-carboxylic acid and 200 mg (0.53 mmol) of HBTU were dissolved in 1.0 mL of DMF and 0.5 mL of DIEA and treated with 200 mg (1.5 mmol) of 2-aminoimidazole sulfate as described in general procedure A. Upon completion, the reaction was diluted with brine. The resulting solid was filtered, washed with water and EtOAc, and dried under vacuum to produce 60 mg (47%) of 6,7-dimethoxy-isoquinoline-3-carboxylic acid [5-ethoxy-7-(1H-imidazol-2-ylcarbamoyl)-1H-benzoimidazol-2-yl]-amide. LCMS: 502 (M+1)+.
후처리
- filtrationThe resulting solid was filtered
- washwashed with water and EtOAc
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-873ab1accd894e268e6a6c2def3fe919
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08598353B2
연결된 노트
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