3'-Hydroxyphenylacetic acid → Ethyl (3-Hydroxyphenyl)acetate
反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([OH:11])=[O:10])[CH:5]=[CH:6][CH:7]=1.O.[C:13]1(C)C=CC(S(O)(=O)=O)=C[CH:14]=1>C(O)C>[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:13][CH3:14])=[O:10])[CH:5]=[CH:6][CH:7]=1参加物
4
実験手順
The stirred solution of 2-(3-Hydroxyphenyl)acetic acid (25 g, 164.3 mmol) and p-Toluenesulfonic acid monohydrate (3.49 g, 18.3 mmol) in abs ethanol (250 ml) was refluxed for 4 hours or until all the starting material is consumed. The reaction mixture was concentrated, diluted with ethyl acetate and washed with 1M HCl. The organic layer was dried over Na2SO4, filtered, concentrated, and purified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1) to give the title compound.
後処理
- customis consumed
- concentrationThe reaction mixture was concentrated
- additiondiluted with ethyl acetate
- washwashed with 1M HCl
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1)
出典と根拠
- ORDレコード
- ord-0a8d1957a73145be91ec799a107852c2
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08829058B2
反応ノート
読み込み中…