반응식
Br[C:2]1[N:6]2[CH2:7][CH2:8][N:9]([C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[C:14]=3[Cl:23])=[O:12])[CH2:10][C:5]2=[N:4][N:3]=1.[Na].[CH3:25][OH:26]>>[Cl:23][C:14]1[C:15]([C:19]([F:22])([F:21])[F:20])=[CH:16][CH:17]=[CH:18][C:13]=1[C:11]([N:9]1[CH2:8][CH2:7][N:6]2[C:2]([O:26][CH3:25])=[N:3][N:4]=[C:5]2[CH2:10]1)=[O:12]참가 물질
실험 절차
3-Bromo-7-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (0.250 g, 0.610 mmol, see Example 1 for methods of preparation) was added to a solution of sodium (0.042 g, 1.831 mmol) in methanol (8 mL), under argon and refluxed for 1 hour. More sodium (0.040 g) was added and the reaction was refluxed for 22 hours. The reaction was quenched with water and extracted with Dichloromethane (three times), the combined organics were dried and evaporated, and the residue was purified on the mass-directed automated (preparative) HPLC (MDAP) and triturated with diethyl ether to give 7-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(methyloxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine (0.082 g) as a white solid.
후처리
- temperaturerefluxed for 1 hour
- temperaturethe reaction was refluxed for 22 hours
- customThe reaction was quenched with water
- extractionextracted with Dichloromethane (three times)
- customthe combined organics were dried
- customevaporated
- customthe residue was purified on the
- customtriturated with diethyl ether
출처 및 근거
- ORD 기록
- ord-701a104241d34d2185bc7fe1ffdb9a31
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08501946B2
연결된 노트
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