Methanol → 1-(Bromomethyl)-2-methanesulfonylbenzene
反応式
CS[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][Br:6].O[O:12][S:13]([O-:15])=O.[K+].[CH3:17]O>O>[CH3:17][S:13]([C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][Br:6])(=[O:15])=[O:12]参加物
5
実験手順
To a solution of 124 mg (0.57 mmol) of 2-(methylthio)-benzylbromide in 8.0 mL of methanol was added a solution of 702 mg of oxone in 7.0 mL of water. The solution was stirred for 4.5 h, concentrated in vacuo and purified by silica gel flash chromatography, eluting with 10% ethyl acetate/hexane to give 105 mg of the title compound. mass spec 249(M+). NMR (CDCl3): δ 3.25 (s, 3H), 5.07 (s, 2H), 7.50 (m, 1H), 7.60 (m, 2H), 8.05 (d, 1H).
後処理
- concentrationconcentrated in vacuo
- custompurified by silica gel flash chromatography
- washeluting with 10% ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-11363b0229f34597bd9f6f342ba64980
- 出典データセット
- uspto-grants-1998_05
- 特許番号
- US05750549
反応ノート
読み込み中…