Hydrochloric Acid → (2-Methanesulfonylphenyl)methanol
反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([CH3:13])(=[O:12])=[O:11].[Li+].[BH4-].Cl>C1COCC1>[CH3:13][S:10]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[CH2:3][OH:2])(=[O:11])=[O:12]参加物
5
実験手順
To a solution of 2-methanesulfonylbenzoic acid methyl ester (1.5 g, 7 mmol) in THF (20 mL) is added LiBH4 (616 mg, 30 mmol) and the mixture is stirred at ambient temperature for 14 h. Additional LiBH4 (310 mg, 15 mmol) is added and the mixture is heated at 65° C. for 45 min. Then under ice cooling, 1N HCl solution is added to quench the excess of LiBH4 before EtOAc is added. The organic layer is washed with brine (2×) and water (1×), dried with MgSO4, and concentrated to give the title compound.
後処理
- temperaturethe mixture is heated at 65° C. for 45 min
- customto quench the excess of LiBH4 before EtOAc
- additionis added
- washThe organic layer is washed with brine (2×) and water (1×)
- dry with materialdried with MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-59f244cf385f488ba5fbbc57ddc7605a
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08119666B2
反応ノート
読み込み中…