4-Bromophenol → 3-(4-Bromophenoxy)oxetane
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].CC1C=CC(S(O[CH:26]2[CH2:29][O:28][CH2:27]2)(=O)=O)=CC=1>CN(C=O)C.CCOC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:26]2[CH2:29][O:28][CH2:27]2)=[CH:4][CH:3]=1参加物
6
反応条件
- 温度
- 100 °C
実験手順
4-Bromophenol (2.5 g, 14.5 mmol) and K2CO3 (5.45 g, 39.4 mmol) were added to a solution of oxetan-3-yl 4-methylbenzenesulfonate (3.00 g, 13.1 mmol) in DMF (10 mL) in a sealed tube. The reaction was heated to 100° C. and stirred at this temperature for 24 h. The reaction was diluted with EtOAc and washed with water. The organic layer was dried (MgSO4), filtered and concentrated to afford the title compound. MS (GCMS) m/z 228. This material was used in subsequent steps without further purification.
後処理
- washwashed with water
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-5eef099f71934001882ac3903275590e
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08624034B2
反応ノート
読み込み中…