Hydroxylamine → 8-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine
반응식
NO.C([N:6](CC)C(C)C)(C)C.[Br:12][C:13]1[C:14]([NH:19][C:20]([NH:22]C(OCC)=O)=S)=[N:15][CH:16]=[CH:17][CH:18]=1>CO.C(O)C>[Br:12][C:13]1[C:14]2[N:15]([N:6]=[C:20]([NH2:22])[N:19]=2)[CH:16]=[CH:17][CH:18]=1참가 물질
6
실험 절차
Hydroxylamine (58.5 g, 842 mmol) and N,N-diisopropylethylamine (65.3 g, 86.3 mL, 505 mmol) were dissolved in methanol (200 mL) and ethanol (200 mL). N-(3-Bromo-pyridin-2-yl)-N′-ethoxycarbonyl-thiourea (51.2 g, 168 mmol) was added and the reaction mixture was stirred at room temperature for 1 hour and then at 60° C. for 3 hours. The white precipitate was filtered off and triturated with water for 25 minutes, filtered and triturated two times with diethylether. The solid was dried by co-evaporation with toluene and dried in vacuum. The title compound was obtained as a white solid (27.9 g, 78%).
후처리
- waitat 60° C. for 3 hours
- filtrationThe white precipitate was filtered off
- customtriturated with water for 25 minutes
- filtrationfiltered
- customtriturated two times with diethylether
- dry with materialThe solid was dried by co-evaporation with toluene
- customdried in vacuum
출처 및 근거
- ORD 기록
- ord-9dd53110377944a686ae91764f37b753
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08486967B2
반응 노트
불러오는 중…