Hydrazine hydrate (1:1) → 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-pyrazole-3-carbohydrazide

HRID 2374452ノート

反応式

HRID 2374452 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21](Cl)=[O:22])[C:9]=2[CH3:24])=[CH:4][CH:3]=1.O.[NH2:26][NH2:27]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([NH:26][NH2:27])=[O:22])[C:9]=2[CH3:24])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 152841395-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carbonyl chloride

生成物 1

HCID 109821545-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-pyrazole-3-carbohydrazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20 g of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carbonyl chloride in 100 ml of ethanol are placed under nitrogen and the mixture is heated at reflux for 2 hours. It is allowed to return to a temperature of 20-25° C., then 50 g of hydrazine hydrate are added and the mixture is again heated at reflux for 3 and a half hours. The reaction medium is filtered while hot and then the ethanol is evaporated. The reaction medium is concentrated, then taken up in 150 ml of DCM and separated by settling. The aqueous phase is discarded, the organic phase is washed twice with 100 ml of water and then the DCM is evaporated. After drying under vacuum, 16.9 g of the expected compound are obtained.

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 2 hours
  3. customto return to a temperature of 20-25° C.
  4. temperaturethe mixture is again heated
  5. temperatureat reflux for 3 and a half hours
  6. filtrationThe reaction medium is filtered while hot and then the ethanol
  7. customis evaporated
  8. concentrationThe reaction medium is concentrated
  9. customseparated
  10. washthe organic phase is washed twice with 100 ml of water
  11. customthe DCM is evaporated
  12. dry with materialAfter drying under vacuum, 16.9 g of the expected compound
  13. customare obtained

出典と根拠

ORDレコード
ord-e76f4285cb0847fc885c32915e454412
出典データセット
uspto-grants-2008_12
特許番号
US07462632B2

反応ノート

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