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Imidazole → HCID 53895873, 화합물

HRID 1153949
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HRID 1153949 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

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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-pentan-2-one in 200 ml of toluene are added to this mixture at 80° C. The reaction mixture is stirred for a further 10 hours at 90° C., cooled and filtered off under suction from the inorganic residue. The filtrate is washed with water, dried over sodium sulphate and evaporated down. 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. temperaturecooled
  2. filtrationfiltered off under suction from the inorganic residue
  3. washThe filtrate is washed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated down
  6. customThe residue is purified by column chromatography (silica gel: ethyl acetate/cyclohexane=3/1)

출처 및 근거

ORD 기록
ord-39b79da91bd0499a88acb27159ff466c
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04487776

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