反应详情

N-Hydroxysuccinimide (0.035 g), followed by 1,3-dicyclohexylcarbodiimide (DCC, 0.064 g), were added to a solution of (S)-1-[(R)-7-(3,5-dichloro-phenyl)-5-methyl-6-oxo-5-(4-pyrimidin-5-yl-benzyl)-6,7-dihydro-5H-imidazo[1,2-a]imidazole-3-sulfonyl]-pyrrolidine-2-carboxylic acid (Example 14) (0.16 g) in CH2Cl2 (20 mL). The reaction was stirred at room temperature for 1 h, then was filtered through a pad of diatomaceous earth, concentrated and re-dissolved in 2N NH3—CH3OH (10 mL). The solution was stirred at room temperature for 1 h. The volatiles were then removed and the resultant residue was re-dissolved in CH2Cl2 and washed with H2O. The combined organic layers were concentrated and the resultant residue was purified by silica gel chromatography to afford the title compound (0.128 g) as a foam (697.2, M+1).

1. filtrationwas filtered through a pad of diatomaceous earth
2. concentrationconcentrated
3. dissolutionre-dissolved in 2N NH3—CH3OH (10 mL)
4. stirringThe solution was stirred at room temperature for 1 h
5. customThe volatiles were then removed
6. dissolutionthe resultant residue was re-dissolved in CH2Cl2
7. washwashed with H2O
8. concentrationThe combined organic layers were concentrated
9. customthe resultant residue was purified by silica gel chromatography