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

HRID 1822893ノート

反応式

HRID 1822893 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
195 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c49bb0db4d86438294f0252143e83318
出典データセット
uspto-grants-2006_05
特許番号
US07037909B2

反応ノート

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