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

HRID 1773975ノート

反応式

HRID 1773975 の反応式
[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]

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-059b8d3803e1430a89e83f9f1a70f243
出典データセット
uspto-grants-2016_02
特許番号
US09255090B2

反応ノート

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