Hydrochloric Acid → Benzeneacetic acid, alpha-ethyl-, methyl ester

HRID 2224920

反応式

HRID 2224920 の反応式
[C:1]1([CH:7]([CH2:11][CH3:12])[C:8]([OH:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[CH3:14]O>>[C:1]1([CH:7]([CH2:11][CH3:12])[C:8]([O:10][CH3:14])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 70122-Phenylbutyric Acid

生成物 1

HCID 102780Benzeneacetic acid, alpha-ethyl-, methyl ester

実験手順

2-Phenylbutyric acid (10 g, 61 mmole) was dissolved in methanol (30 ml) treated with concentrated HCl (1 ml) and heated at reflux for 20 hours. The heating was stopped and the reaction mixture cooled to room temperature. The solvent was removed in vacuo and the oily residue was treated with ethyl acetate (100 ml). The organic layer was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a clear oil. Yield 10.61 g (97%). 1H NMR (300 MHz, DMSO-d6): δ ppm 0.81 (t, J=7.35 Hz, 3 H) 1.69 m, 1 H) 1.98 (m, 1 H) 3.53 (d, J=7.35 Hz, 1 H) 3.58 (s, 3 H) 7.30 m, 5 H).

後処理

  1. temperatureheated
  2. temperatureat reflux for 20 hours
  3. customThe solvent was removed in vacuo
  4. additionthe oily residue was treated with ethyl acetate (100 ml)
  5. washThe organic layer was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3f62aa99713645f1982eb32bb8ac8e6b
出典データセット
uspto-grants-2008_05
特許番号
US07378414B2

関連ノート

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