反应详情

温度

65 °C

A 22 L, three-necked round bottom flask equipped with an air-powered mechanical stirrer was placed under a nitrogen atmosphere. The vessel was charged with methyl valerimidate hydrochloride (2.5 kg, 16 mol) and dimethylformamide (9.2 L). A thermometer was attached and the suspension cooled to 0°-15° C. with a cooling bath. Triethylamine (2.3 L) was added to the reaction at such a rate so that the internal temperature did not exceed 25° C. The cooling was stopped and the reaction was allowed to stir 1 hour. The reaction mixture was vacuum filtered using a Buchner funnel and a carboy (20 L). The filter cake was washed with additional dimethylformamide (1.0 L) and force-air dried for 15 min. The combined filtrates were saved. Another clean 22 L, three-necked round bottom flask equipped as above was placed under nitrogen. The vessel was charged with the combined filtrates from above followed by triethylamine (1.6 L) and 4-(aminomethyl)benzoic acid (1.7 kg, 11.5 mol). The thermometer was attached and the suspension was heated to an internal temperature of 65° C. with a heating mantle and a temperature controller. The heating was continued for 20 hours. The reaction was cooled to ambient temperature and filtered to yield 2.5 kg of product; 92% uncorrected yield.

1. customA 22 L, three-necked round bottom flask equipped with an air-powered mechanical stirrer
2. temperaturethe suspension cooled to 0°-15° C. with a cooling bath
3. customdid not exceed 25° C
4. filtrationfiltered
5. washThe filter cake was washed with additional dimethylformamide (1.0 L)
6. customforce-air dried for 15 min
7. customAnother clean 22 L, three-necked round bottom flask equipped
8. additionThe vessel was charged with the combined filtrates
9. waitThe heating was continued for 20 hours
10. temperatureThe reaction was cooled to ambient temperature
11. filtrationfiltered