HCID 22125181, 화합물 → HCID 22125045, 화합물
반응식
[NH:1]([C:8]1[N:13]=[C:12]2[N:14]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([CH2:33][CH2:34]OS(C)(=O)=O)[CH:28]=3)[C:15](=[O:26])[N:16]([C:18]3[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:25])[CH2:17][C:11]2=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:40]1(=[O:50])[NH:44][C:43](=[O:45])[C:42]2=[CH:46][CH:47]=[CH:48][CH:49]=[C:41]12.[K]>CN(C)C=O>[NH:1]([C:8]1[N:13]=[C:12]2[N:14]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([CH2:33][CH2:34][N:44]4[C:40](=[O:50])[C:41]5=[CH:49][CH:48]=[CH:47][CH:46]=[C:42]5[C:43]4=[O:45])[CH:28]=3)[C:15](=[O:26])[N:16]([C:18]3[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:25])[CH2:17][C:11]2=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
4
반응 조건
- 온도
- 90 °C
실험 절차
A solution of 233 mg (0.41 mmol) of 7-anilino-3-(2-chloro-6-methylphenyl)-3,4-dihydro-1-[3-(2-methanesulfonyloxyethyl)phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one in 10 ml of dimethylformamide was treated with 100 mg (0.54 mmol) of potassium phthalimide and the mixture heated at 90° C. for 3 hours. The mixture was cooled and evaporated. The residue was partitioned between 50 ml of ethyl acetate and 50 ml of water. The organic phase was dried over magnesium sulfate, filtered and evaporated to give 250 mg (99%) of 7-anilino-3-(2-chloro-6-methylphenyl)-3,4-dihydro-1-[3-(2-phthalimidoethyl)phenyl]-pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid. [Mass spectrum (ESI) MH+ =615].
후처리
- temperatureThe mixture was cooled
- customevaporated
- customThe residue was partitioned between 50 ml of ethyl acetate and 50 ml of water
- dry with materialThe organic phase was dried over magnesium sulfate
- filtrationfiltered
- customevaporated
출처 및 근거
- ORD 기록
- ord-f771b07057db4de19b79032e42443ed0
- 출처 데이터셋
- uspto-grants-2000_11
- 특허 번호
- US06150373
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