反应详情

温度

-15 °C

1.86 Milliliters of N-methylmorpholine was dissolved in 60 ml of tetrahydrofuran and to this solution 4.85 g of Z-Leu-OH was added. The mixture was cooled to -15° C. and 2.41 ml of isobutyl chloroformate was added and then vigorously stirred for 30 seconds. To this reaction mixture, 40 ml of a dimethylformamide solution containing 2.54 g of H-Gly-OC2H5, and 2.56 ml of triethylamine were added and stirred for 1 minute. After the reaction mixture was warmed at 0° C. for 5 minutes, then at 40° C. for 2 minutes and was stirred at a room temperature for 15 minutes. Tetrahydrofuran and dimethylformamide were removed by distillation to obtain the residue, then 1M-citric acid was added to this residue and the crystals thus formed were collected by filtration. The crystals were washed with water until the filtrate become neutral, and the crystals were dried, reprecipitated from ethyl acetate-ether to obtain 4.68 g of Z-Leu-Gly-OC2H5.

1. additionwas added
2. additionwere added
3. stirringstirred for 1 minute
4. temperatureAfter the reaction mixture was warmed at 0° C. for 5 minutes
5. waitat 40° C. for 2 minutes
6. stirringwas stirred at a room temperature for 15 minutes
7. customTetrahydrofuran and dimethylformamide were removed by distillation
8. customto obtain the residue
9. customthe crystals thus formed
10. filtrationwere collected by filtration
11. washThe crystals were washed with water until the filtrate
12. customthe crystals were dried
13. customreprecipitated from ethyl acetate-ether