反応式
Cl.Cl.[NH2:3][CH2:4][CH2:5][CH2:6][S:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1.C(N(CC)CC)C.[C:21]([Cl:27])(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]>C(Cl)Cl>[ClH:27].[C:21]([NH:3][CH2:4][CH2:5][CH2:6][S:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]参加物
5
実験手順
To a solution of 1.00 g (4.15 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.77 ml (19.8 mmol) of triethylamine in 40 ml of methylene chloride was added 0.61 ml (4.96 mmol) of pivaloyl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 1.01 g of the desired compound (free base) (96.4%, yellow oil).
後処理
- temperaturecooling
- stirringthe mixture was stirred at room temperature for 30 minutes
- washThe reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water
- customdried
- distillationThe 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-4c449e2f33634ee381298abe83df1119
- 出典データセット
- uspto-grants-1998_06
- 特許番号
- US05767121
関連ノート
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