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

HRID 451459

反応式

HRID 451459 の反応式
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

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

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

  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

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

関連ノート

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