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

HRID 128454

반응식

HRID 128454 반응식
[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

참가 물질

4

반응물 2

HCID 7516PhenylhydrazineHCID 12569643N-Dimethylaminomethylene-isonicotinamide

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0a98110ee36f40d5b1f1c8b0c4729bee
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259504

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