Triethylamine → 4-(3-Hydroxypropylthio)pyridine
反応式
[SH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.Br[CH2:16][CH2:17][CH2:18][OH:19]>C(Cl)Cl>[OH:19][CH2:18][CH2:17][CH2:16][S:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1参加物
5
実験手順
In 100 ml of methylene chloride were dissolved 11.1 g (100 mmol) of 4-mercaptopyridine and 13.9 ml (100 mmol) of triethylamine, and 9.04 ml (100 mmol) of 3-bromo-1-propanol was added. The mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water and dried. Then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 14.2 g of the desired compound (yield: 83.9%, yellow oil).
後処理
- additionwas added
- washThe reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water
- customdried
- distillationThen the solvent was distilled off
- customThe residue was purified by column chromatography (eluent: ethyl acetate)
出典と根拠
- ORDレコード
- ord-e97eadac01b44ac8865f4b6513251185
- 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…