반응식
[N:1]1C=CN2CCNCC=12.ClC1NC(=[O:21])[C:18]2[C:13](=[CH:14][C:15](OC)=[C:16](OC)[CH:17]=2)N=1.[N:26]1[CH:27]=[CH:28][N:29]2[CH2:34][CH2:33][N:32]([C:35]3[NH:36][C:37]4[C:42]([C:43](=[O:45])[N:44]=3)=[CH:41][C:40]([O:46][CH3:47])=[C:39]([O:48][CH3:49])[CH:38]=4)[CH2:31][C:30]=12.BrC1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[NH4+:1].[OH-:21].[CH3:47][O:46][C:40]1[CH:41]=[C:42]2[C:37](=[CH:38][C:39]=1[O:48][CH3:49])[NH:36][C:35]([N:32]1[CH2:33][CH2:34][N:29]3[C:28]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)=[CH:27][N:26]=[C:30]3[CH2:31]1)=[N:44][C:43]2=[O:45]참가 물질
10
반응물 6
생성물 2
시약·촉매·용매 2
반응 조건
- 온도
- 140 °C
실험 절차
5,6,7,8-Tetrahydro-imidazo[1,2-a]pyrazine, prepared as described in PCT Application WO 01/44250, was coupled with 2-chloro-6,7-dimethoxy-3H-quinazolin-4-one 1b, as described herein. 2-(5,6-dihydro-8H-imidazo[1,2-a]pyrazin-7-yl)-6,7-dimethoxy-1H-quinazolin-4-one (150 mg, 0.46 mmol) was combined with bromobezene (97 μL, 0.92 mmol), potassium carbonate (127 mg, 0.92 mmol), palladium acetate (5 mg, 5 mol %), and triphenylphosphine (13 mg, 10 mol %) in DMF (6 mL). The mixture was heated in a 140° C. bath for 2 d, then concentrated onto silica gel followed by eluting with 300:10:1 CH2Cl2:MeOH:NH4OH) to afford 50 mg of 6,7-dimethoxy-2-(3-phenyl-5,6-dihydro-8H-imidazo[1,2-α]pyrazin-7-yl)-1H-quinazolin-4-one, 904, mp: >300° C, M+=403.
후처리
- concentrationconcentrated onto silica gel
- washby eluting with 300:10:1 CH2Cl2
출처 및 근거
- ORD 기록
- ord-6647c4f09b6c419a9d4dc6d55a619a4e
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091200B2
연결된 노트
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