Dimethyl Sulfoxide → Benzenemethanol, alpha-ethenyl-, 1-acetate

HRID 1983976

반응식

HRID 1983976 반응식
[CH:1]([CH:3](Cl)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[CH2:2].[C:11]([O-:14])(=[O:13])[CH3:12].[K+].CS(C)=O>O>[C:11]([O:14][CH:3]([CH:1]=[CH2:2])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:13])[CH3:12]

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 517044Potassium AcetateHCID 11768772Benzene, 1-(chloromethyl)-3(or 4)-ethenyl-

생성물 1

HCID 111277Benzenemethanol, alpha-ethenyl-, 1-acetate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

In a one liter 3-neck round bottom flask equipped with a condenser, mechanical stirrer and thermometer, 108 grams (0.708 mol) of vinylbenzyl chloride (60/40 m-/p-) and 808 grams (0.815 mol) of potassium acetate were added, followed by 250 mLs of DMSO. The mixture was stirred at 40° C. for 48 hours. After allowing to cool to room temperature, the mixture was diluted with water and poured into a separatory funnel. The organic layer was separated, followed by an extraction of the aqueous layer with chloroform. The combined organic layer was then washed with water, dried over magnesium sulfate and placed on the rotary evaporator to remove the chloroform. 120 grams of the vinylbenzyl acetate product was recovered, to which 10 mg of MEHQ was added as an inhibitor.

후처리

  1. customIn a one liter 3-neck round bottom flask equipped with a condenser, mechanical stirrer
  2. temperatureto cool to room temperature
  3. additionpoured into a separatory funnel
  4. customThe organic layer was separated
  5. extractionfollowed by an extraction of the aqueous layer with chloroform
  6. washThe combined organic layer was then washed with water
  7. dry with materialdried over magnesium sulfate
  8. customplaced on the rotary evaporator
  9. customto remove the chloroform
  10. custom120 grams of the vinylbenzyl acetate product was recovered, to which 10 mg of MEHQ
  11. additionwas added as an inhibitor

출처 및 근거

ORD 기록
ord-af0c0b19934242bfaa47c6791779d4f5
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544453B2

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