Methyl iodide → Methyl 2-(3-bromo-2-methoxyphenyl)acetate

HRID 1773975노트

반응식

HRID 1773975 반응식
[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Br:11])[C:6]=1[OH:12].[C:14](=O)([O-])[O-].[K+].[K+].IC>CC#N.CCOC(C)=O.O>[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Br:11])[C:6]=1[O:12][CH3:14]

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 12159074Methyl 2-(3-bromo-2-hydroxyphenyl)acetate

생성물 1

HCID 66643982Methyl 2-(3-bromo-2-methoxyphenyl)acetate

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

To a solution of (3-bromo-2-hydroxy-phenyl)-acetic acid methyl ester (866 mg, 3.5 mmol, 1 eq.) and potassium carbonate (2.44 g, 17.7 mmol, 5 eq.) in MeCN (9 mL), iodomethane (0.67 mL, 10.6 mmol, 3 eq.) was added. The resulting mixture was stirred at 50° C. for 2 hours. The reaction mixture was diluted with AcOEt and water. The layers were separated and the aq. phase was extracted with AcOEt (2×). The comb. org. layers were dried over MgSO4, filtered, and concentrated in vacuo to give the title compound as an orange oil. The product was used without further purification.

후처리

  1. customThe layers were separated
  2. extractionthe aq. phase was extracted with AcOEt (2×)
  3. dry with materiallayers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-059b8d3803e1430a89e83f9f1a70f243
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09255090B2

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