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Water → 1-(2,4-difluorophenyl)-2-(1H-pyrazol-1-yl)ethanone

HRID 1531404
ノート
印刷プレビュー

反応式

HRID 1531404 の反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[F:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[C:14](=[O:17])[CH2:15]Cl.O>CC(C)CC(=O)C>[F:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[C:14](=[O:17])[CH2:15][N:1]1[CH:5]=[CH:4][CH:3]=[N:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 1048PyrazoleHCID 5880832-Chloro-1-(2,4-difluorophenyl)ethanone

生成物 1

HCID 212539981-(2,4-difluorophenyl)-2-(1H-pyrazol-1-yl)ethanone収率 78%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒2 回

実験手順

A mixture of 1H-pyrazole (1.3 mol) in 4-methyl-2-pentanone (500 ml) was stirred and refluxed. 1-(2,4-difluorophenyl)-2-chloroethanone (0.26 mol) dissolved in 4-methyl-2-pentanone (500 ml) was added dropwise and the mixture was stirred and refluxed for 3 h. The mixture was cooled, poured into water and separated. The organic layer was evaporated. The residue was stirred up in HCl/water, filtered off and washed with water. The precipitate was stirred up in hexane, filtered off and dried in vacuo at 45° C., yielding 45 g (78%) of 1-(2,4-difluorophenyl)-2-(1H-pyrazol-1-yl)ethanone; mp. 76.4° C. (interm. 12).

後処理

  1. temperaturerefluxed
  2. additionwas added dropwise
  3. stirringthe mixture was stirred
  4. temperaturerefluxed for 3 h
  5. temperatureThe mixture was cooled
  6. customseparated
  7. customThe organic layer was evaporated
  8. stirringThe residue was stirred up in HCl/water
  9. filtrationfiltered off
  10. washwashed with water
  11. stirringThe precipitate was stirred up in hexane
  12. filtrationfiltered off
  13. customdried in vacuo at 45° C.

出典と根拠

ORDレコード
ord-2c7c320a0c414e0d9332e5903a5a333f
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06197972B1

反応ノート

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