反应详情

温度

61 °C

A mixture of 5-Chloro-2-hydroxy-3-methoxybenzaldehyde (275 g, 1.47 mol) and DMF were stirred as potassium carbonate (411 g, 2.97 mol) was added over 5 minutes. The mixture temperature rose from 22 to 29° C. over 10 minutes. Dimethylsulfate (283 g, 2.24 mol) was added over 15 minutes causing a temperature rise from 28 to 47° C. The mixture was then heated with a heating mantle to 61° C. over 15 minutes and stirred at 61° C. for 1.5 hours; the reaction was complete by TLC. The reaction mixture was cooled to 22° C., transferred to a 22-L flask and diluted with water (8.2 L) over 5 minutes; the temperature rose to 38° C. The light yellow mixture was filtered and the flask and filter cake rinsed with 1.5 L water. The solid was dried under vacuum for 15 hour at 50° C. The material contained inorganic salts and was suspended in water (3 L) for 1.5 hours. After filtration and a 500 mL water rinse, the filter cake was dried under by suction and overnight at 65° C. under vacuum. Yield: 305 g (100% yield, 99.1% purity).

1. additionwas added over 5 minutes
2. customfrom 28 to 47° C
3. temperatureThe reaction mixture was cooled to 22° C.
4. customtransferred to a 22-L flask
5. customrose to 38° C
6. filtrationThe light yellow mixture was filtered
7. filtrationthe flask and filter cake
8. washrinsed with 1.5 L water
9. customThe solid was dried under vacuum for 15 hour at 50° C
10. waitwas suspended in water (3 L) for 1.5 hours
11. filtrationAfter filtration
12. washa 500 mL water rinse
13. customthe filter cake was dried under by suction and overnight at 65° C. under vacuum