Hydroxylamine → 8-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine
反応式
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]=1参加物
6
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-9dd53110377944a686ae91764f37b753
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08486967B2
反応ノート
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