反应详情

In 2 ml of DMF were dissolved 300 mg of Nα -[(S)-2-azetidinone-4-carbonyl]-L-histidyl-L-proline (13) (obtained in Example 3), 116 mg of HOBT, and 177 mg of DCC and after stirring for 7 hours at room temperature, the solution was cooled in an ice bath. Then 0.6 ml of a methanol solution of 30% methylamine was added to the solution and the mixture was reacted overnight with stirring at 2° to 6° C. Insoluble matters were filtered off and the filtrate was concentrated to dryness under reduced pressure. The residue thus formed was purified by column chromatography using LiChroprep Si 60(size B). By using chloroform-methanol-aqueous ammonia (40:10:1) as the eluant, Nα -[(S)-2-azetidinone-4-carbonyl]-L-histidyl-N-methyl-L-prolinamide (46) was obtained. The product was dissolved in water and then lyophilized. The amount of the product thus obtained was 149 mg.

1. temperaturethe solution was cooled in an ice bath
2. customthe mixture was reacted overnight
3. stirringwith stirring at 2° to 6° C
4. filtrationInsoluble matters were filtered off
5. concentrationthe filtrate was concentrated to dryness under reduced pressure
6. customThe residue thus formed
7. customwas purified by column chromatography