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

HRID 1586367노트

반응식

HRID 1586367 반응식
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]

참가 물질

7

반응물 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 178478181HCID 178478181, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9e665cd2e424891badd17a2fe583bd7
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05945382

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