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

HRID 128454

反応式

HRID 128454 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 orange 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 orange 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-0a98110ee36f40d5b1f1c8b0c4729bee
出典データセット
uspto-grants-1981_03
特許番号
US04259504

関連ノート

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