Phosphorus tribromide → 1-(Bromomethyl)-2-methanesulfonylbenzene
反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11]O)(=[O:4])=[O:3].P(Br)(Br)[Br:14]>C(Cl)Cl.C([O-])(O)=O.[Na+]>[Br:14][CH2:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[S:2]([CH3:1])(=[O:4])=[O:3]参加物
5
実験手順
To a stirred solution of (2-methanesulfonyl-phenyl)methanol (735 mg, 3.99 mmol) in dry DCM (2 mL) at 0° C., add a solution of 1M phosphorous tribromide in DCM (6.0 mL, 6.0 mmol) and continue stirring for 1 h. Dilute with saturated aqueous NaHCO3, extract three times with ethyl ether, dry over anhydrous MgSO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (12:1) to provide the title compound as a white solid (950 mg, 97%).
後処理
- extractionextract three times with ethyl ether
- dry with materialdry over anhydrous MgSO4
- concentrationconcentrate in vacuo
- customPurify by chromatography on silica gel eluting with hexane/EtOAc (12:1)
出典と根拠
- ORDレコード
- ord-d17ca875288a47e6856302733baa2767
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08580780B2
反応ノート
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