Hydrazine → 5-[(4-Fluorophenyl)methyl]-4H-1,2,4-triazole-3,4-diamine

HRID 1822893노트

반응식

HRID 1822893 반응식
[F:1][C:2]1[CH:14]=[CH:13][C:5]([CH2:6][C:7]2O[C:10]([NH2:12])=[N:9][N:8]=2)=[CH:4][CH:3]=1.[NH2:15][NH2:16]>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][C:7]2[N:15]([NH2:16])[C:10]([NH2:12])=[N:9][N:8]=2)=[CH:13][CH:14]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 219193195-[(4-Fluorophenyl)methyl]-1,3,4-oxadiazol-2-amine

생성물 1

HCID 219193225-[(4-Fluorophenyl)methyl]-4H-1,2,4-triazole-3,4-diamine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
195 °C

실험 절차

A mixture of 5-(4-fluoro-benzyl)-[1,3,4]oxadiazol-2-ylamine 10.182 g (52.7 mmol), water 80 mL and anhydrous hydrazine 20 mL was refluxed under nitrogen on an oil bath (190-200° C.) for 23 hours. The mixture was cooled and allowed to crystallize at room temperature under nitrogen overnight. The precipitated product was collected by filtration, washed with ice-cold water (10 mL) and dried on high vacuum. The crude product was re-crystallized from water 60 mL (reflux under nitrogen, than to +4° C. in a refrigerator overnight). The product was filtered, washed with ice-cold water and dried on high vacuum.

후처리

  1. temperatureThe mixture was cooled
  2. customto crystallize at room temperature under nitrogen overnight
  3. filtrationThe precipitated product was collected by filtration
  4. washwashed with ice-cold water (10 mL)
  5. customdried on high vacuum
  6. customThe crude product was re-crystallized from water 60 mL (
  7. temperaturereflux under nitrogen, than to +4° C. in a refrigerator overnight)
  8. filtrationThe product was filtered
  9. washwashed with ice-cold water
  10. customdried on high vacuum

출처 및 근거

ORD 기록
ord-c49bb0db4d86438294f0252143e83318
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07037909B2

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