Water → 1-Acetyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole

HRID 1586367ノート

反応式

HRID 1586367 の反応式
C(N(CC)CC)C.[Cl:8][C:9]1[C:10]([C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)=[N:11][NH:12][CH:13]=1.[C:22](Cl)(=[O:24])[CH3:23].O>CN(C)C1C=CN=CC=1.C1COCC1>[C:22]([N:12]1[CH:13]=[C:9]([Cl:8])[C:10]([C:14]2[CH:15]=[C:16]([Cl:21])[CH:17]=[C:18]([Cl:20])[CH:19]=2)=[N:11]1)(=[O:24])[CH3:23]

参加物

7

反応物 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 178478181HCID 178478181、化合物

生成物 1

HCID 218526591-Acetyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole収率 96.7%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.35 g (0.003 mol) of 4-dimethylaminopyridine and 1.55 ml (0.011 mol) of triethylamine are added to 2.55 g (0.01 mol) of 4-chloro-3-(3,5-dichlorophenyl)-pyrazole dissolved in 30 ml of THF. A solution of 0.85 g (0.011 mol) of acetyl chloride in 10 ml of THF is run, dropwise and at 0° C., onto this solution. Stirring is continued for 2 h at room temperature. The reaction mixture is poured into 100 ml of water and extracted with ethyl acetate. After drying the organic phase and concentration under vacuum, the residue is triturated with 50 ml of heptane, filtered and dried. We obtain 2.80 g of 1-acetyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole, melting at 125° C.

後処理

  1. customat 0° C.
  2. extractionextracted with ethyl acetate
  3. customAfter drying
  4. concentrationthe organic phase and concentration under vacuum
  5. customthe residue is triturated with 50 ml of heptane
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-b9e665cd2e424891badd17a2fe583bd7
出典データセット
uspto-grants-1999_08
特許番号
US05945382

反応ノート

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