Bromine → 1-(4-Bromothiophen-2-yl)-2-methylpropan-1-one
反応式
[CH3:1][CH:2]([CH3:10])[C:3]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)=[O:4].[Cl-].[Al+3].[Cl-].[Cl-].[Br:15]Br>C(Cl)(Cl)Cl>[Br:15][C:8]1[CH:9]=[C:5]([C:3](=[O:4])[CH:2]([CH3:10])[CH3:1])[S:6][CH:7]=1参加物
5
実験手順
2-methyl-1-(2-thienyl)-1-propanone (2.3 g, 15 mmol) was diluted in chloroform (10 mL), and aluminum chloride (4.5 g, 34 mmol, 2.3 eq) was added. Bromine (0.82 mL, 16 mmol, 1.1 eq) was added as a solution in chloroform (15 mL), and the mixture was stirred at rt over the weekend. The crude reaction mixture was carefully poured onto ice water, then extracted with chloroform. The combined organics were dried over sodium sulfate, filtered, and concentrated to afford brown oil. The crude was purified by isco combiflash to give the title compound as brown oil (1.28 g, 40%).
後処理
- customThe crude reaction mixture
- additionwas carefully poured onto ice water
- extractionextracted with chloroform
- dry with materialThe combined organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto afford brown oil
- customThe crude was purified by isco combiflash
出典と根拠
- ORDレコード
- ord-6e82853107d04ec6ae5b57c01e3c76bc
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071584B2
反応ノート
読み込み中…