反应详情

温度

90 °C

A mixture of Na2S.9H2O (65 g, 0.28 mol), sulfur (25 g, 0.78 mol) and water (150 mL) were heated with stirring at 90° C. for 10 min, and then poured into a flask charged with the above 4′-chloro-3′-nitroacetanilide (21.5 g, 0.10 mol). The resulting mixture was heated at 80° C. for 10 min, and then CS2 (12 mL, 0.2 mol) was added dropwise while maintaining a gentle reflux. The resulting mixture was heated at 90° C. for 7 h. The solids were collected by filtration, washed with water and dilute HCl solution. The solids were taken up in water, and the solution was made alkaline with solid NaOH. The solution was filtered, and the filtrate was acidified with conc HCl. The precipitates were collected by filtration, washed with water, and dried under high vacuum. The crude product was suspended in cold water (200 mL) and solid Na2CO3 was added to obtain pH 13. Dimethyl sulfate was added to the above milky solution, and the resulting mixture was stirred at ambient temperature for 3 h. The solids were collected by filtration, washed with water, and dried under high vacuum to yield the title compound (12.4 g, 55%).

1. temperaturewere heated
2. additionpoured into a flask
3. temperatureThe resulting mixture was heated at 80° C. for 10 min
4. temperaturewhile maintaining a gentle reflux
5. temperatureThe resulting mixture was heated at 90° C. for 7 h
6. filtrationThe solids were collected by filtration
7. washwashed with water and dilute HCl solution
8. filtrationThe solution was filtered
9. filtrationThe precipitates were collected by filtration
10. washwashed with water
11. customdried under high vacuum
12. additionsolid Na2CO3 was added
13. customto obtain pH 13
14. stirringthe resulting mixture was stirred at ambient temperature for 3 h
15. filtrationThe solids were collected by filtration
16. washwashed with water
17. customdried under high vacuum