Ethyl Acetate → HCID 23042157、化合物

HRID 2166101ノート

反応式

HRID 2166101 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11](O)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](=[O:18])([O-])[O-].[K+].[K+].[Br:21][C:22]1[S:23][CH:24]=[C:25](CCl)[CH:26]=1.C(OCC)(=O)C>CN(C)C=O>[Br:21][C:22]1[S:23][CH:24]=[C:25]([CH2:15][O:18][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[O:1][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:26]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 132544-PhenoxyphenolHCID 128741092-Bromo-4-(chloromethyl)thiophene

生成物 1

HCID 23042157HCID 23042157、化合物収率 113.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

7.44 g of 4-phenoxyphenol and 5.52 g of potassium carbonate are stirred in 50 ml of anhydrous dimethylformamide for 1 hour at 70° C. 5.52 g of 2-bromo-4-chloromethylthiophene is then dripped in, and the mixture is stirred for a further 12 hours at 80° C., and at room temperature (approx. 20° C.) overnight. The mixture is then stirred into 500 ml of ethyl acetate and washed three times with water. After drying over sodium sulfate and removal of the solvent, the residue is recrystallized from n-hexane. There is obtained 10.7 g of 2-bromo-4-[(phenoxyphenoxy)-methyl]-thiophene; colorless powder; m.p.: 90° C.

後処理

  1. customat room temperature
  2. custom(approx. 20° C.) overnight
  3. washwashed three times with water
  4. dry with materialAfter drying over sodium sulfate and removal of the solvent
  5. customthe residue is recrystallized from n-hexane

出典と根拠

ORDレコード
ord-ec1b8f9b6ccb498997b34037395a1d9a
出典データセット
uspto-grants-1990_07
特許番号
US04943584

反応ノート

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