Bromine → 2-Isopropylsulphinylbenzaldehyde
反応式
[CH:1]([S:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=[O:8])([CH3:3])[CH3:2].BrBr.[O-:15]S([O-])=O.[Na+].[Na+]>ClCCl>[CH:1]([S:4]([C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=[O:8])=[O:15])([CH3:3])[CH3:2]参加物
5
実験手順
A solution of 2-(isopropylthio)benzaldehyde (0.33 g, 1.83 mmol) in dichloromethane (10 ml) was admixed with aqueous KHCO3 solution (1.18 g in 10 ml of H2O). With vigorous stirring, a solution of bromine (0.310 g, 1.93 mmol) in dichloromethane (1.5 ml) was added dropwise. After continuing to stir for 20 min, a spatula-tip of Na2SO3 was added, and the organic phase was removed, washed with saturated NaCl solution, dried over MgSO4 and filtered, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (3:1 to 1:1 hexane:ethyl acetate). The product precipitated out as a yellowish oil. Yield 0.304 g (85%).
後処理
- customthe organic phase was removed
- washwashed with saturated NaCl solution
- dry with materialdried over MgSO4
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customThe residue was purified by column chromatography on silica gel (3:1 to 1:1 hexane:ethyl acetate)
- customThe product precipitated out as a yellowish oil
出典と根拠
- ORDレコード
- ord-cbae1d996ed64f209cb2b016cb6a8f15
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183382B2
反応ノート
読み込み中…