Methanol → Methyl 2-(3-fluoro-4-hydroxyphenyl)acetate
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[OH:8].[CH3:13]O.S(=O)(=O)(O)O>O>[CH3:13][O:11][C:10](=[O:12])[CH2:9][C:4]1[CH:5]=[CH:6][C:7]([OH:8])=[C:2]([F:1])[CH:3]=1参加物
5
実験手順
A mixture of 2.0 g of 3-fluoro-4-hydroxybenzeneacetic acid, 10 ml of methyl alcohol and 1 ml of concentrated sulfuric acid is heated at reflux temperature for 23.5 hours. The cooled solution is diluted with water and extracted with methylene chloride. The organic layer is washed with water, saturated sodium bicarbonate, water and saturated sodium chloride; dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:25% ethyl acetate/hexane) to give 1.9 g of the desired product.
後処理
- temperatureis heated
- temperatureat reflux temperature for 23.5 hours
- extractionextracted with methylene chloride
- washThe organic layer is washed with water, saturated sodium bicarbonate, water and saturated sodium chloride
- customdried
- concentrationconcentrated in vacuo
- customThe residue is purified by column chromatography (silica gel:25% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-1b4c5b4238094374b404e5e81d4d6beb
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05208247
反応ノート
読み込み中…