Triethylamine → 4-(4-Chlorobutylthio)pyridine
反応式
[SH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.Br[CH2:9][CH2:10][CH2:11][CH2:12][Cl:13].C(N(CC)CC)C>C(O)C>[Cl:13][CH2:12][CH2:11][CH2:10][CH2:9][S:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1参加物
5
実験手順
To a suspension of 33.35 g (0.30 mol) of 4-mercaptopyridine and 51.44 g (0.30 mol) of 1-bromo-4-chlorobutane in 500 ml of ethanol, 41.9 ml (0.30 mol) of triethylamine was added, and the mixture was stirred at room temperature for 5 hours. The solvent was distilled off and chloroform was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane =1:1) to give 54.27 g of the desired compound (89.7% yield, colorless oil).
後処理
- additionwas added
- distillationThe solvent was distilled off
- additionchloroform was added to the residue
- washThe mixture was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off
- customthe residue was purified by column chromatography (eluent: ethyl acetate/n-hexane =1:1)
出典と根拠
- ORDレコード
- ord-4aaaa3a6821445dabee298f6b50af2bd
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05246948
反応ノート
読み込み中…