反应详情

温度

4 °C

Methylamine (146.1 grams; 4.70 moles) contained in 40% aqueous methyl amine solution (365.4 grams) was placed in a 3-liter, 3-necked glass reaction flask equipped with addition funnel, stirrer, thermometer and reflux condenser and containing ether (1200 ml) cooled to 4° C. 2-methoxy-3,6-dichlorobenzoic acid chloride (375 grams; 1.56 moles) in ether (50 ml) was added dropwise with stirring maintaining the temperature below 8° C. After the completion of the addition the reaction mixture was stirred for an additional two hours at a temperature of between 2° and 5° C. The insoluble white solid was filtered with suction, washed with water, transferred to a 3-liter beaker and stirred fifteen (15) minutes with 10% sodium carbonate (2 liters). The insoluble white solid was filtered with suction, washed with water and dried. The product weighed 352 grams and had a melting point of 172.5°-175° C.

1. customwas placed in a 3-liter, 3-necked glass reaction flask
2. customequipped with addition funnel, stirrer
3. temperaturethermometer and reflux condenser
4. temperaturemaintaining the temperature below 8° C
5. additionAfter the completion of the addition the reaction mixture
6. stirringwas stirred for an additional two hours at a temperature of between 2° and 5° C
7. filtrationThe insoluble white solid was filtered with suction
8. washwashed with water
9. stirringstirred fifteen (15) minutes with 10% sodium carbonate (2 liters)
10. filtrationThe insoluble white solid was filtered with suction
11. washwashed with water
12. customdried