反应详情

Glycine methyl ester hydrochloride was suspended in tetrahydrofuran, the suspension was cooled to -5° C. to -10° C., and then half of the N-methylmorpholine was added. Cinnamoyl chloride was added immediately, followed by the other half of the N-methylmorpholine. The reaction mixture was stirred for 30 minutes at low temperature, then it was allowed to warm to room temperature and stirring was continued for 2 to 3 hours. After being diluted with ethyl acetate (about 750 ml) the solution was washed with water (three times), an aqueous solution of 0.5 N hydrochloric acid (three times) and finally with water. The organic phase was dried over magnesium sulfate, filtered and evaporated to dryness under reduced pressure. The residue was triturated with petroleum ether is order to induce crystallization. The product was left to stand for about 14 hours at 4° C., then it was filtered off and dried in a vacuum. It was used in the next step without further purification. 31 g of product were obtained.

1. temperaturethe suspension was cooled to -5° C. to -10° C.
2. stirringstirring
3. waitwas continued for 2 to 3 hours
4. washwas washed with water (three times)
5. dry with materialThe organic phase was dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated to dryness under reduced pressure
8. customThe residue was triturated with petroleum ether
9. customcrystallization
10. waitThe product was left
11. waitto stand for about 14 hours at 4° C.
12. filtrationit was filtered off
13. customdried in a vacuum
14. customIt was used in the next step without further purification