反应详情

温度

0 °C

A reaction of indomethacin (1.79 g, 5.00 mmol) and the product of Example 91 (0.830 g, 5.00 mmol) was carried out, using dicyclohexylcarbodiimide (1.10 g, 5.50 mmol) as the coupling agent and acetonitrile as the solvent. The first two reactants were dissolved completely and the solution was then cooled to 0° C. The dicyclohexylcarbodiimide was added and the mixture was stirred overnight. The reaction was allowed to continue for 48 hours. The precipitate (1.2 g) was removed by vacuum filtration. The solvent was removed from the filtrate under reduced pressure leaving an oily residue. The product was solidified by stirring with anhydrous ether. It was filtered, air-dried and recrystallized from ethanol/ether. The final product was vacuum filtered, washed with ether, and air dried. The product weighed 1.65 g, giving a 65.2% yield; mp 123°-125° C.

1. dissolutionThe first two reactants were dissolved completely
2. waitto continue for 48 hours
3. customThe precipitate (1.2 g) was removed by vacuum filtration
4. customThe solvent was removed from the filtrate under reduced pressure
5. customleaving an oily residue
6. filtrationIt was filtered
7. customair-dried
8. customrecrystallized from ethanol/ether
9. filtrationfiltered
10. washwashed with ether, and air
11. customdried
12. customgiving a 65.2% yield