Hydrochloric Acid → Methyl 3-methoxy-5-sulfanylbenzoate
反応式
[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[C:6]([S:12]C(=O)N(C)C)[CH:5]=1.CO[Na].Cl>C1COCC1>[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[C:6]([SH:12])[CH:5]=1参加物
5
実験手順
To a stirred solution of 3-dimethylcarbamylthio-5-methoxybenzoic acid methyl ester (500 mg, 1.86 mmol) in THF (10 mL) at room temperature was added MeONa (0.5 M in MeOH, 10.0 mL, 5.0 mmol, 2.69 eq.). The reaction was refluxed for 2 h, then cooled to room temperature and added to 1.0 N HCl aqueous solution (150 mL). The resulting mixture was extracted with EtOAc/hexanes (1:1, 150 mL). The organic layer was washed with brine (100 mL), dried over MgSO4 and concentrated in vacuo to give 3-mercapto-5-methoxybenzoic acid methyl ester (0.365 g). The product was used without further purification.
後処理
- temperatureThe reaction was refluxed for 2 h
- extractionThe resulting mixture was extracted with EtOAc/hexanes (1:1, 150 mL)
- washThe organic layer was washed with brine (100 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-4a6fb25a094740a0998572628d8d55dd
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07691843B2
反応ノート
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