Phenylhydrazine → 4-(1-Phenyl-1H-1,2,4-triazol-5-yl)pyridine

HRID 1065486

反応式

HRID 1065486 の反応式
[C:1]1([NH:7][NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN([CH:12]=[N:13][C:14](=O)[C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1)C>C(O)(=O)C>[C:1]1([N:7]2[C:14]([C:15]3[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=3)=[N:13][CH:12]=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 7516PhenylhydrazineHCID 12569643N-Dimethylaminomethylene-isonicotinamide

生成物 1

HCID 128502974-(1-Phenyl-1H-1,2,4-triazol-5-yl)pyridine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

To a solution of 6.9 g. of phenylhydrazine in 100 ml. of acetic acid is added 10.0 g. of N-(dimethylaminomethylene)-isonicotinamide. The reaction mixture is stirred at 90° C. for 1.5 hours and then evaporated in vacuo to an organce oil. This oil is dissolved in 250 ml. of chloroform, washed with 60 ml. of saturated sodium bicarbonate solution, then with 60 ml. of water, dried over sodium sulfate and filtered. The chloroform is removed and the residue is dissolved in 60 ml. of ether. Cooling produces 8.8 g. of the desired product as tan crystals, mp. 92°-94° C.

後処理

  1. customevaporated in vacuo to an organce oil
  2. dissolutionThis oil is dissolved in 250 ml
  3. washof chloroform, washed with 60 ml
  4. dry with materialof water, dried over sodium sulfate
  5. filtrationfiltered
  6. customThe chloroform is removed
  7. dissolutionthe residue is dissolved in 60 ml
  8. temperatureCooling
  9. customproduces 8.8 g

出典と根拠

ORDレコード
ord-aa3c2fab56cd493ca92f44a4ee5c03d1
出典データセット
uspto-grants-1982_05
特許番号
US04329463

関連ノート

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