Water → HCID 57431971、化合物
反応式
[CH3:1][O:2][C:3](=[O:14])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11]C)=[CH:7][C:6]=1[CH3:13].[Cl-].[Al+3].[Cl-].[Cl-].C(S)C.O>ClCCl>[CH3:1][O:2][C:3](=[O:14])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[CH3:13]参加物
6
実験手順
(4-Methoxy-2-methyl-phenyl)-acetic acid methyl ester (1.5 g, 7.72 mmol) is stirred in dichloromethane (50 mL) at 0 deg. C. Aluminum chloride (4.13 g, 31 mmol) is added followed by ethane thiol (2.9 mL, 38.6 mmol). The resulting mixture is stirred at room temperature for 2 hr. Water (50 mL) is added and the product is extracted into ethyl acetate (3×50 ml), the extracts are combined, dried over anhydrous magnesium sulfate, filtered, and concentrated to afford the title compound as a colorless oil, 1.4 g, 100%. MS M++1 181. The structure is confirmed by 1H NMR spectroscopy.
後処理
- extractionthe product is extracted into ethyl acetate (3×50 ml)
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-179282a82ad1468d84a34c38efea4ddc
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07259175B2
反応ノート
読み込み中…