Methanol → (R)-Methyl 2-(2-chlorophenyl)-2-hydroxyacetate
反応式
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C@@H:4]([OH:8])[C:5]([OH:7])=[O:6].P(=O)(Cl)(Cl)Cl.[CH3:18]O>>[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C@@H:4]([OH:8])[C:5]([O:7][CH3:18])=[O:6]参加物
4
実験手順
15 g of (R)-2-chloromandelic acid was mixed with methanol (CH3OH, 150 ml) and phosphorus chloride oxide (POCl3, 0.76 ml) in a flask by stirring using a magnetic stirrer at the room temperature for 6 hours. When the reaction was completed, the obtained product was washed with an aqueous solution of sodium sulfite (Na2SO3) and ethylacetate (EA). Then, the organic layer was dehydrated with anhydrous magnesium sulfate (MgSO4), filtrated, and concentrated under reduced pressure. The concentrated residue was purified by a silica gel column chromatography to produce the title compound (15.64 g, yield 95%).
後処理
- customat the room temperature
- customfor 6 hours
- washthe obtained product was washed with an aqueous solution of sodium sulfite (Na2SO3) and ethylacetate (EA)
- filtrationfiltrated
- concentrationconcentrated under reduced pressure
- customThe concentrated residue was purified by a silica gel column chromatography
出典と根拠
- ORDレコード
- ord-25129f185ee64f75bede769f0a90c2d3
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859817B2
反応ノート
読み込み中…