Ethyl Acetate → HCID 23042157, 화합물

HRID 2166101노트

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HRID 2166101 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 23042157HCID 23042157, 화합물수율 113.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec1b8f9b6ccb498997b34037395a1d9a
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04943584

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