Hydroxylamine → 8-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine

HRID 451459

반응식

HRID 451459 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]=1

참가 물질

6

반응물 3

HCID 787HydroxylamineHCID 81531DiisopropylethylamineHCID 59199107Ethyl aminon-(3-bromopyridin-2-YL)methanethiocarbamate

생성물 1

HCID 468640698-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

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

  1. waitat 60° C. for 3 hours
  2. filtrationThe white precipitate was filtered off
  3. customtriturated with water for 25 minutes
  4. filtrationfiltered
  5. customtriturated two times with diethylether
  6. dry with materialThe solid was dried by co-evaporation with toluene
  7. customdried in vacuum

출처 및 근거

ORD 기록
ord-9dd53110377944a686ae91764f37b753
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

연결된 노트

불러오는 중…