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Imidazole → HCID 53895873, 화합물

HRID 464391
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HRID 464391 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH:13]([O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1)[C:14](=[O:21])[C:15]([CH3:20])([CH3:19])[CH2:16][CH2:17]Cl>C1(C)C=CC=CC=1>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([O:22][C:13]([N:1]2[CH:5]=[CH:4][N:3]=[CH:2]2)=[C:14]2[C:15]([CH3:20])([CH3:19])[CH2:16][CH2:17][O:21]2)=[CH:24][CH:25]=1
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참가 물질

5

반응물 3

HCID 795ImidazoleHCID 11430Potassium CarbonateHCID 132542811-Bromo-5-chloro-1-(4-chlorophenoxy)-3,3-dimethylpentan-2-one

생성물 1

HCID 53895873HCID 53895873, 화합물수율 15.9%

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
90 °C

실험 절차

35 g (0.5 mol) of imidazole and 70 g (0.5 mol) of potassium carbonate are dissolved in 700 ml of toluene. 93 g (0.26 mol) of 1-bromo-1-(4-chlorophenoxy)-5-chloro-3,3-dimethyl-2-pentanone in 200 ml of toluene are added to this mixture at 80° C. The reaction mixture is subsequently stirred at 90° C. for 10 hours and is cooled and the inorganic residue is filtered off with suction. The filtrate is washed with water, dried over sodium sulphate and concentrated. The residue is purified by column chromatography (silica gel: ethyl acetate/cyclohexane=3/1). 12.6 g (14.2% of theory) of (4-chlorophenoxy)-(imidazol-1-yl)-(3,3-dimethyltetrahydrofuran-2-ylidene)-methane of melting point 85°-88° C. are obtained.

후처리

  1. temperatureis cooled
  2. filtrationthe inorganic residue is filtered off with suction
  3. washThe filtrate is washed with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. customThe residue is purified by column chromatography (silica gel: ethyl acetate/cyclohexane=3/1)

출처 및 근거

ORD 기록
ord-b7e7e93e754040ed803dee3e9ed206eb
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04547515

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