反応式
[H-].[Na+].[C:3](#[N:7])[CH2:4][C:5]#[N:6].[CH3:8][N:9]=[C:10]=[S:11].[CH3:12]I>CN(C)C=O>[C:5]([C:4]([C:3]#[N:7])=[C:10]([S:11][CH3:12])[NH:9][CH3:8])#[N:6]参加物
実験手順
Sodium hydride (50% oil dispersion, 9.6 g) was added portionwise to a solution of malononitrile (13.21 g) in dry dimethylformamide (150 ml). The mixture was stirred at 0° for 10 minutes and then to it was added dropwise a solution of methyl isothiocyanate (14.62 g) in dimethylformamide, maintaining the reaction temperature below 40°. The dark red solution was stirred for 45 minutes and a solution of methyl iodide (28.4 g) in dimethylformamide (25 ml) was then added. The reaction mixture was stirred vigorously for 20 minutes and then poured on to crushed ice (500 ml). The crude product (26 g, m.p. 115°) was filtered off and taken up in hot ethanol ether (3:1, 600 ml). Filtration and cooling furnished 1,1-dicyano-2-methylthio-2-methylamino ethylene m.p. 119°-120°. Further recrystallisation from water gave a sample of m.p. 120°-121°.
後処理
- temperaturemaintaining the reaction temperature below 40°
- stirringThe dark red solution was stirred for 45 minutes
- stirringThe reaction mixture was stirred vigorously for 20 minutes
- additionpoured on
- filtrationThe crude product (26 g, m.p. 115°) was filtered off
- filtrationFiltration
- temperaturecooling
出典と根拠
- ORDレコード
- ord-444c2c0140f64e58917c37308e4d6a38
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04220652
関連ノート
読み込み中…