反应详情

Phenyl 6-(2-chloro-4-iodophenylamino)-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate (Example 23, 300 mg, 0.588 mmol, 1 eq) and (R)—O-((2,2-dimethyl-1,3-dioxolan-4-yl)methyl)hydroxylamine (260 mg, 1.826 mmol, 3 eq) were mixed in anhydrous THF (1.5 ml). The mixture was subjected to microwave irradiation at 100° C. for 50 minutes. The intended product was isolated by HPLC purification to give 140 mg of white solid (42%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.38 (s, 3H) 1.46 (s, 3H) 3.04 (s, 3H) 3.38 (s, 3H) 3.85-3.8758 (m, J=8 Hz, 1H) 4.03-4.05 (d, J=8 Hz, 2H) 4.10-4.11 (t, J=4Hz, 1H) 6.70-6.72 (d, J=8 Hz, 1H) 7.56-7.58 (d, J=8 Hz, 1H) 7.82 (s, 1H) 12.07 (s, 1H) 12.79 (s, 1H) [M+H] calc'd for C19H22ClIN4O6, 565; found, 565.

1. customirradiation at 100° C. for 50 minutes
2. customThe intended product was isolated by HPLC purification