反应详情

In 8 ml of DMF was dissolved 277 mg of compound (13) and then 168 mg of HOBT and 330 mg of DCC were added to the solution under ice-cooling. After maintaining a reaction for one hour under ice-cooling, the reaction was further maintained for 2 hours at room temperature. After ice-cooling again the reaction mixture, 2 ml of a DMF solution of 80 mg of monoethanolamine to maintain the reaction for one hour and thereafter, the reaction was further maintained overnight at room temperature. The precipitates were filtered off, the filtrate was concentrated to dryness, and the residue thus formed was dissolved in 10 ml of chloroform-methanol-aqueous ammonia (40:10:1) and subjected to silica gel column chromatography. Then, the product was eluted with the same solvent as above to provide 106 mg of Nα -[(S)-2-azetidinone-4-carbonyl]-L-histidyl-N-(2-hydroxyethyl)-L-prolinamide (14).

1. temperaturecooling
2. temperatureAfter maintaining
3. customa reaction for one hour under ice-
4. temperaturecooling
5. temperatureto maintain
6. customthe reaction for one hour
7. temperaturethe reaction was further maintained overnight at room temperature
8. filtrationThe precipitates were filtered off
9. concentrationthe filtrate was concentrated to dryness
10. customthe residue thus formed
11. washThen, the product was eluted with the same solvent as above