Methanol → 2-(4-Bromo-phenyl)-5-chloropentanoic acid methyl ester
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH2:12][CH2:13][CH2:14][Cl:15])[C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[CH3:16]O>O=S(Cl)Cl>[CH3:16][O:10][C:9](=[O:11])[CH:8]([C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=1)[CH2:12][CH2:13][CH2:14][Cl:15]参加物
4
実験手順
To a solution of 2-(4-Bromo-phenyl)-5-chloropentanoic acid (3 g, 10.38 mmol) in MeOH (60 mL), SOCl2 (2 mL) was added at 0 degrees Celsius, then the mixture refluxed for 5 h. After cooling, the solution was evaporated to dryness under reduced pressure, then EtOAc was added and the mixture was washed with aq. NaHCO3, the organic layer was dried with MgSO4, and evaporated to give the compound as an oil (2.85 g, 90%). MS: calc'd 304 (MH+), exp 304 (MH+).
後処理
- temperaturethe mixture refluxed for 5 h
- temperatureAfter cooling
- customthe solution was evaporated to dryness under reduced pressure
- additionEtOAc was added
- washthe mixture was washed with aq. NaHCO3
- dry with materialthe organic layer was dried with MgSO4
- customevaporated
出典と根拠
- ORDレコード
- ord-29d22aa1221447b0b06b96161033fd5f
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202866B2
反応ノート
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