Dimethyl Sulfate → Ethyl 4-methoxyphenylacetate

HRID 446805

반응식

HRID 446805 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][CH:3]=1.[C:14]([O-])([O-])=O.[K+].[K+].COS(OC)(=O)=O>C(#N)C>[CH3:14][O:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 28310Ethyl 4-hydroxyphenylacetate

생성물 1

HCID 84174Ethyl 4-methoxyphenylacetate수율 91,530.898%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of ethyl 2-(4-hydroxyphenyl)acetate (15 g, 0.09 mmol) in acetonitrile (100 mL) were added anhydrous K2CO3 (27.23 g, 0.19 mol) followed by Me2SO4 (14.94 g, 0.11 mol) at RT. The reaction mixture was then refluxed for 5 h, filtered through a pad of Celite® and the filtrate was concentrated in vacuo. The residue was dissolved in EtOAc (300 mL). The organic layer was then washed with water, dried over Na2SO4 and concentrated in vacuo to afford ethyl 2-(4-methoxyphenyl)acetate (16 g, 84%) as a solid.

후처리

  1. temperatureThe reaction mixture was then refluxed for 5 h
  2. filtrationfiltered through a pad of Celite®
  3. concentrationthe filtrate was concentrated in vacuo
  4. dissolutionThe residue was dissolved in EtOAc (300 mL)
  5. washThe organic layer was then washed with water
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-64d293839418460b9b70e3330194fa9f
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481534B2

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