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[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH:25]1([NH2:31])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1>>[CH:25]1([NH:31][C:14]2[N:15]=[CH:16][C:11]3[CH:10]=[C:9]([C:3]4[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=4[Cl:8])[C:22](=[O:23])[N:21]([CH3:24])[C:12]=3[N:13]=2)[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1참가 물질
3
반응 조건
- 온도
- 134 °C
실험 절차
A mixture of 0.100 g (0.26 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.300 g (3.00 mmol) of cyclohexylamine was heated to the boiling point (134° C.). The resulting solution was heated at reflux for 2 minutes. Most of the excess amine was evaporated at reduced pressure. The remaining gum was dissolved in 2 mL of ethyl acetate hot. Petroleum ether (2 mL) was added, and the crystals that separated from the cooled solution were filtered and washed with water; wt 0.090 g. Recrystallization from ethyl acetate gave pure crystalline product; 0.048 g; mp 242°-244° C.
후처리
- temperatureThe resulting solution was heated
- temperatureat reflux for 2 minutes
- customMost of the excess amine was evaporated at reduced pressure
- dissolutionThe remaining gum was dissolved in 2 mL of ethyl acetate hot
- additionPetroleum ether (2 mL) was added
- customthe crystals that separated from the cooled solution
- filtrationwere filtered
- washwashed with water
- customRecrystallization from ethyl acetate
- customgave pure crystalline product
출처 및 근거
- ORD 기록
- ord-3191b5ba687c4a38ba69160188ee969d
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05733914
연결된 노트
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