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Potassium Carbonate → (Z)-4-[4-(2-Imidazol-1-yl-ethoxy)phenyl]-3,4-diphenyl-but-3-en-1-ol

HRID 1368937
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반응식

HRID 1368937 반응식
Br[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8](/[C:11](/[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:12](\[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)/[CH2:13][CH2:14][OH:15])=[CH:7][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].[Na].[NH:35]1[CH:39]=[CH:38][N:37]=[CH:36]1>C(C(C)=O)C>[N:35]1([CH2:2][CH2:3][O:4][C:5]2[CH:10]=[CH:9][C:8](/[C:11](/[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[C:12](\[C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)/[CH2:13][CH2:14][OH:15])=[CH:7][CH:6]=2)[CH:39]=[CH:38][N:37]=[CH:36]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 57373095Imidazole sodiumHCID 69544510Z-1,2-diphenyl-1-[4-(bromoethoxy)phenyl]-1-buten-4-ol

생성물 1

HCID 69545262(Z)-4-[4-(2-Imidazol-1-yl-ethoxy)phenyl]-3,4-diphenyl-but-3-en-1-ol

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

(Z)-4-[4-(2-Bromoethoxy)phenyl]-3,4-diphenylbut-3-en-1-ol (preparation described in U.S. Pat. No. 4,996,225) (4.97 g, 0.0117 mol) is dissolved in methyl ethyl ketone (50 ml) and potassium carbonate (4.8 g, 0.035 mol) and imidazole sodium salt (2.1 1 g, 0.0234 mol) is added to the solution. Mixture is stirred and refluxed for five hours. Then the solution is filtered and the filtrate is evaporated to dryness. The residue is dissolved in ethyl acetate, washed with 2 N aqueous sodium hydroxide solution and with water, dried and evaporated to dryness. The residue is recrystallized from the mixture of toluene and acetonitrile.

후처리

  1. temperaturerefluxed for five hours
  2. filtrationThen the solution is filtered
  3. customthe filtrate is evaporated to dryness
  4. dissolutionThe residue is dissolved in ethyl acetate
  5. washwashed with 2 N aqueous sodium hydroxide solution and with water
  6. customdried
  7. customevaporated to dryness
  8. customThe residue is recrystallized from the mixture of toluene and acetonitrile

출처 및 근거

ORD 기록
ord-09aec0aefdfa4d7382da0b1871bcd746
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06576645B1

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