Benzene → 4-(2,4-Dichlorobenzoyl)-1-methyl-5-(p-acetylbenzyloxy)pyrazole

HRID 637595

반응식

HRID 637595 반응식
C1C=CC=CC=1.[Cl:7][C:8]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:9]=1[C:10]([C:12]1[CH:13]=[N:14][N:15]([CH3:18])[C:16]=1[OH:17])=[O:11].[C:24]([C:27]1[CH:34]=[CH:33][C:30]([CH2:31]Br)=[CH:29][CH:28]=1)(=[O:26])[CH3:25]>C(N(CC)CC)C>[Cl:7][C:8]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:9]=1[C:10]([C:12]1[CH:13]=[N:14][N:15]([CH3:18])[C:16]=1[O:17][CH2:31][C:30]1[CH:33]=[CH:34][C:27]([C:24](=[O:26])[CH3:25])=[CH:28][CH:29]=1)=[O:11]

참가 물질

5

반응물 3

HCID 241BenzeneHCID 5837851-[4-(Bromomethyl)phenyl]ethan-1-oneHCID 178481842HCID 178481842, 화합물

생성물 1

HCID 155907284-(2,4-Dichlorobenzoyl)-1-methyl-5-(p-acetylbenzyloxy)pyrazole수율 83%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

In 30 ml of dry benzene containing 0.50 g (0.005 mol) of triethylamine was dissolved 1.36 (0.005 mol) of 4-(2,4-dichlorobenzoyl)-1-methyl-5-hydroxypyrazole, and then 1.07 g (0.005 mol) of p-acetylbenzylbromide was added thereto. The resulting mixture was heated under reflux for 3 hours. After cooling the reaction mixture, the salt precipitated was filtered off and the solvent was distilled off therefrom under reduced pressure. The resulting oil was purified through column chromatography on silica gel using benzene/ethyl acetate 8:1 as an eluent to give 1.67 g of the title compound (yield 83%).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling the reaction mixture
  4. customthe salt precipitated
  5. filtrationwas filtered off
  6. distillationthe solvent was distilled off
  7. customThe resulting oil was purified through column chromatography on silica gel

출처 및 근거

ORD 기록
ord-70c3c8650efc4dc0acd3abc0a8cb70b0
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04557753

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