反应详情

Oxalyl chloride (190 mg; 1.5 mmol) was added to a suspension of Intermediate 15 (144 mg; 0.5 mmol) and DMF (catalytic amount) in DCM (2 mL) and the reaction mixture was stirred at RT for 1 hour. After concentration to dryness, the residue was taken up in THF (2 mL) and added to a solution of 4-(aminosulfonyl)-N′-hydroxybenzenecarboximidamide, prepared as described in WO 2006/013104 A1 from 4-cyanobenzene-1-sulfonamide (ABCR; CD10716), (108 mg; 05 mmol, 1 eq.) and DIEA (194 mg; 1.5 mmol) in THF (1 mL). The reaction mixture was then stirred at 150° C. for 30 minutes in the microwave. After cooling, the mixture was filtered through a SPE-NH2 column, which was further washed with THF. After concentration in vacuo, the residue was purified by recrystallisation from DCM/n-pentane, affording the title compound as a white solid. LC/MS (Method A): 467.3 (M+H)+. HPLC (Method A) Rt 5.59 min (purity 99.3%).

1. concentrationAfter concentration to dryness
2. additionadded to a solution of 4-(aminosulfonyl)-N′-hydroxybenzenecarboximidamide
3. customprepared
4. stirringThe reaction mixture was then stirred at 150° C. for 30 minutes in the microwave
5. temperatureAfter cooling
6. filtrationthe mixture was filtered through a SPE-NH2 column, which
7. washwas further washed with THF
8. concentrationAfter concentration in vacuo
9. customthe residue was purified by recrystallisation from DCM/n-pentane