反应详情

温度

0 °C

A solution of acetic acid 2-{1-[2-amino-3-(4-fluorophenyl)propionyl]-4-(1-methylcarbamoyl-2-naphthalen-2-ylethyl)piperazin-2-yl}-ethyl ester, 64, (54.9 g, 100 mmol), hydroxybenzotriazole (16.2 g, 120 mmol), and N-methylmorpholine (132 mL, 120 mmol) in DMF (150 mL) is cooled to 0° C. and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (24.9 g, 130 mmol) is slowly added. The resulting mixture is stirred for 2 hours at 0° C. then allowed to warm and stir at room temperature another 2 hours. The reaction solution is diluted with water and the resulting solid is collected by filtration, re-dissolved in EtOAc and extracted with water, dried and concentrated in vacuo to afford a residue which purified over silica gel.

1. temperatureto warm
2. stirringstir at room temperature another 2 hours
3. filtrationthe resulting solid is collected by filtration
4. dissolutionre-dissolved in EtOAc
5. extractionextracted with water
6. customdried
7. concentrationconcentrated in vacuo
8. customto afford a residue which
9. custompurified over silica gel