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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
ノート
印刷プレビュー

反応式

HRID 1368937 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-09aec0aefdfa4d7382da0b1871bcd746
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06576645B1

反応ノート

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