Dichloromethane → HCID 676779, Verbindung
Reaktionsgleichung
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](Br)[N:3]=1.[CH2:9]([O:11][C:12]([N:14]=[C:15]=[S:16])=[O:13])[CH3:10].Cl[CH2:18]Cl>>[CH2:9]([O:11][C:12](=[O:13])[NH:14][C:15](=[S:16])[NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:18])[N:3]=1)[CH3:10]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 24 °C
Versuchsvorschrift
To an ice-cooled solution of 2-amino-6-bromopyridine (25.0 g, 0.144 mmol, 1 equiv) in dichloromethane (400 mL) was added ethoxycarbonyl isothiocyanate (19.9 g, 0.152 mmol, 1.05 equiv) dropwise. The reaction mixture was warmed to 24° C. After 21 h, the reaction mixture was concentrated in vacuo (˜20 mm Hg). The residue was diluted with ethyl acetate (600 mL), and the resulting organic solution was washed sequentially with water (2×200 mL) and saturated aqueous sodium chloride solution (200 mL). The organic was dried over magnesium sulfate, filtered, and concentrated to afford product as a yellow solid (43.7 g).