Diethyl Ether → HCID 178509637、化合物

HRID 708948

反応式

HRID 708948 の反応式
[N+]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:14]=[CH:13][NH:12][N:11]=2)=[CH:6][CH:5]=1)([O-])=O.[C:15](C1C=CC(C(N)=O)=CC=1)#[N:16].O.NN.CCOCC>CN(C(OC)OC)C>[NH:12]1[CH:13]=[N:14][C:10]([C:7]2[CH:8]=[CH:9][C:4]([C:15]#[N:16])=[CH:5][CH:6]=2)=[N:11]1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 24654Hydrazine hydrate (1:1)HCID 76427p-CyanobenzamideHCID 178526551HCID 178526551、化合物

生成物 1

HCID 178509637HCID 178509637、化合物

試薬・触媒・溶媒 1

HCID 78373Dimethylformamide dimethyl acetal溶媒

実験手順

The general procedure outlined by Lin et al. (J. Org. Chem. 1979, 44, 4163) for preparation of 3-(4-nitrophenyl)-1H-[1,2,4]triazole was used. 4-Cyanobenzamide (21.63 g, 0.148 mol) was dissolved in DMF-DMA (100 mL) and was stirred at reflux under N2 for 8 h. The mixture was concentrated to dryness and suspended in AcOH (50 mL). The vessel was then charged with hydrazine monohydrate (7.18 mL, 0.148 mmol) and stirred at reflux for 1 h before concentration. The desired 4-(1H-[1,2,4]triazol-3-yl)-benzonitrile was obtained in 98% purity by trituration with Et2O followed by filtration (12.17 g, 0.072 mol, 48%).

後処理

  1. temperatureat reflux under N2 for 8 h
  2. concentrationThe mixture was concentrated to dryness
  3. stirringstirred
  4. temperatureat reflux for 1 h before concentration

出典と根拠

ORDレコード
ord-7ecbca45bacd4186a67ae60fe0beea32
出典データセット
uspto-grants-2015_11
特許番号
US09179681B2

関連ノート

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