反应详情

温度

160 °C

A mixture of 1000 mg (4.35 mmol) N-amino-N′,N″-dimethyl-guanidine hydriodide (Henry; Smith; J. Amer. Chem. Soc.; 73; 1951; 1858) and 774 mg (4.35 mmol) isonicotinoyl chloride hydrochloride in pyridine (3 mL) was heated under microwave irradiation for 5 min at 160° C. Aq. sat. K2CO3 was added and the mixture was extracted with CHCl3. The organic phase was dried and concentrated. Recrystallization from EtOH, water and EA gave 216 mg (26%) of the title compound. 1H NMR (DMSO-d6): 2.85 (d, 3 H) 3.45 (s, 3 H) 6.25 (d, 1 H) 7.65 (m, 2 H) 8.67 (m, 2 H).

1. extractionthe mixture was extracted with CHCl3
2. customThe organic phase was dried
3. concentrationconcentrated
4. customRecrystallization from EtOH, water and EA