反応式
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][OH:6].[O:7]1[CH:12]=[CH:11][CH2:10][CH2:9][CH2:8]1.C(=O)([O-])[O-].[K+].[K+]>ClCCl.P(Cl)(Cl)(Cl)=O>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][O:6][CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12][O:7]1参加物
6
実験手順
To a solution of commercially available 4-bromobutan-1-ol (16) (1 equi.) and 3,4-dihydropyran (17) (1.5 equi.) in dichloromethane (3 mL/mmole), phosphorus oxychloride (0.01 equi.) was added at room temperature. The reaction mixture was stirred at that temperature for 24 h. Then potassium carbonate (1 equi.) was added to the reaction mixture and the reaction mixture was stirred at room temperature for 1 h, quenched with water, extracted with dichloromethane, washed with brine, dried over MgSO4, and concentrated in vacuo. Purification by chromatography on silica gel (5% EtOAc/hexanes) afforded 2-(4-bromobutoxy)-tetrahydropyran (18), as a colorless oil (88%).
後処理
- stirringthe reaction mixture was stirred at room temperature for 1 h
- customquenched with water
- extractionextracted with dichloromethane
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customPurification by chromatography on silica gel (5% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-897b02d40a5c415e94fa7c6fe1ac97fb
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07083832B2
関連ノート
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