反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[N:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][NH:1][S:17]([CH3:16])(=[O:19])=[O:18]参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a 0° solution of 15 g of 2-(aminomethyl)pyridine, 15.44 g of triethylamine and 150 ml of methylene chloride is added 17.48 g of methanesulfonyl chloride in 100 ml of methylene chloride. The mixture is stirred at 0° C. for 1 hour followed by stirring at room temperature for 3 hours. The reaction is poured into saturated sodium bicarbonate and extracted with methylene chloride. The combined extracts are washed with saturated sodium chloride and concentrated in vacuo. The residue is purified by chromatography (silica gel: 10% methyl alcohol/ethyl acetate) to give 19.84 g of the desired product.
後処理
- stirringby stirring at room temperature for 3 hours
- extractionextracted with methylene chloride
- washThe combined extracts are washed with saturated sodium chloride
- concentrationconcentrated in vacuo
- customThe residue is purified by chromatography (silica gel: 10% methyl alcohol/ethyl acetate)
出典と根拠
- ORDレコード
- ord-9e181e15af8d430ab55c46ae28c7b1fb
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05208247
関連ノート
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