反应详情

To methyl 3-[2-(2,6-dichlorophenyl)-6-quinolinyl]-2-[(2-isopropoxy-3,4-dioxo-1-cyclobuten-1-yl)amino]propanoate 116 (690 mg) in CH3OH (20 ml) are added 132 μl of n-propylamine. After addition of DMF (15 ml), the solution is stirred at RT overnight. The evaporation of CH3OH gives a DMF residue that is diluted in water (200 ml) and stirred overnight. The solid is filtered, washed with water then with MeOH, diluted in DMF, and n-propylamine (150 μl) is added to drive the reaction to completion. The solution is stirred at RT for 48 h, then poured into water. DMF is evaporated and the resulting solid is filtered, washed with water and dried. The product is purified by HPLC/MS (eluent: CH3CN/water/TFA, 8 minutes gradient from respectively 5/95/0.1 to 95/5/0.1). CH3CN is evaporated and water is added to the residue. The resulting solid is filtered and dried to give methyl 3-[2-(2,6-dichlorophenyl)-6-quinolinyl]-2-{[3,4-dioxo-2-(propylamino)-1-cyclobuten-1-yl]amino}propanoate 123.

1. customThe evaporation of CH3OH
2. customgives a DMF residue that
3. stirringstirred overnight
4. filtrationThe solid is filtered
5. washwashed with water
6. additionwith MeOH, diluted in DMF
7. additionn-propylamine (150 μl) is added
8. customthe reaction to completion
9. stirringThe solution is stirred at RT for 48 h
10. customDMF is evaporated
11. filtrationthe resulting solid is filtered
12. washwashed with water
13. customdried
14. customThe product is purified by HPLC/MS (eluent
15. customCH3CN/water/TFA, 8 minutes
16. customCH3CN is evaporated
17. additionwater is added to the residue
18. filtrationThe resulting solid is filtered
19. customdried