Water → HCID 15581961、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8]([NH2:10])=[S:9].O.[CH2:12](N)[C:13]#[CH:14]>C(O)C>[CH2:14]([NH:10][C:8](=[S:9])[CH2:7][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1)[C:13]#[CH:12]参加物
5
実験手順
To 4.0 g. (0.026 mole) of 2-(2-pyridyl)thioacetamide in 20 ml. of water at 0°C. is added 2.9 g. (0.053 mole) of propargylamine with stirring and the resulting suspension is allowed to stand overnight at 5°C. Ethanol (5 ml.) is added and the mixture is stirred for 5 hours, then extracted with dichloromethane. The extracts are dried and concentrated. The residue is chromatographed on a silica gel "dry-column", using 1:10 ethyl acetate/ether as the eluant. The product fraction is treated with charcoal, filtered, concentrated and the residue is recrystallized from benzene/ligroin to give N-propargyl-2-(2-pyridyl)thioacetamide, m.p. 62°-63°C.
後処理
- extractionextracted with dichloromethane
- customThe extracts are dried
- concentrationconcentrated
- customThe residue is chromatographed on a silica gel "dry-column"
- additionThe product fraction is treated with charcoal
- filtrationfiltered
- concentrationconcentrated
- customthe residue is recrystallized from benzene/ligroin
出典と根拠
- ORDレコード
- ord-d6815c441f864c4b957d2033197b9f1f
- 出典データセット
- uspto-grants-1976_04
- 特許番号
- US03950522
反応ノート
読み込み中…