反应详情

The title compound was obtained according to the procedure described for the synthesis of Example 24, starting from 5-chloro-N-hexyl-2,4-dioxo-pyrimidine-1-carboxamide (Example 3) (0.119 g, 0.431 mmol); 2.4 equivalents of isobutyl chloroformate were used herein. The crude was purified by column chromatography using a Teledyne ISCO apparatus (cyclohexane:EtOAc 85:15) to afford the title compound (0.047 g, 29%) as a white solid. 1H NMR (400 MHz, CDCl3): δ 0.89 (t, J=6.8 Hz, 3H), 1.01 (d, J=6.7 Hz, 6H), 1.28-1.38 (m, 6H), 1.57-1.64 (m, 2H), 2.11 (h, J=6.7 Hz, 1H), 3.39 (td, J=7.1, 5.5, 2H), 4.26 (d, J=6.6, 2H), 8.62 (s, 1H), 8.80 (t, J=4.9 Hz, 1H). 13C NMR (101 MHz, CDCl3): δ 14.12, 18.89 (2C), 22.63, 26.58, 27.81, 29.19, 31.48, 41.77, 76.77, 111.14, 135.14, 148.40, 148.58, 149.20, 156.04. MS (ESI) m/z: 391 [M-NH4]+.

1. customdescribed for the synthesis of Example 24
2. customThe crude was purified by column chromatography