反应详情

356 g (3.4 mols+14% excess) of maleic acid monomethyl ester are placed into a glass flask provided with stirrer, thermometer, condenser and dropping funnel, and, with vigorous stirring and ice-water cooling, 480 ml of triethylamine are added dropwise at 5°-8° C. internal temperature within 2 hours. 372.6 g (2.4 mols) of 3-cyclohexylaminopropylamine are then quickly introduced; the exothermic reaction is subsequently allowed to subside, and the reaction mixture is heated within 30 minutes to 85° C., in the course of which the reaction product crystallises out. After the reaction has finished, the temperature is lowered to room temperature; the product is mixed with 1100 ml of acetone and is filtered off; the filter residue is again mixed with 900 ml of acetone, and the suspension is filtered; the filter residue is then washed with acetone, and the product is dried at 60° C. and 53.2 mbars. The yield is 555.4 g (87.2% of theory) of a white crystalline aspartic acid derivative, which decomposes at 163° C.

1. customprovided with stirrer
2. customthermometer, condenser and dropping
3. customthe exothermic reaction
4. temperaturethe reaction mixture is heated within 30 minutes to 85° C., in the course of which the reaction product
5. customcrystallises out
6. customis lowered to room temperature
7. additionthe product is mixed with 1100 ml of acetone
8. filtrationis filtered off
9. additionthe filter residue is again mixed with 900 ml of acetone
10. filtrationthe suspension is filtered
11. washthe filter residue is then washed with acetone
12. customthe product is dried at 60° C.
13. customdecomposes at 163° C.