反应详情

温度

140 °C

{(R)-2-[5-bromo-3-(2,6-difluoro-benzyl)-4-methyl-2,6-dioxo-3,6-dihydro-2H-pyrimidin-1-yl]-1-phenyl-ethyl}-carbamic acid tert-butyl ester (100 mg, 0.182 mmol) and piperazine-2-one (187 mg, 1.82 mmol) were placed into a microwave flask along the wall of which 1 mL of acetonitrile was then added. The solution was stirred at 140° C. for 3 hrs while being irradiated with microwaves. After concentration in a vacuum, the concentrate was purified by column chromatography eluting with a dichloromethane/methanol (35/1) eluent to afford 60 mg of the compound as a yellowish solid (yield 58%). 1H NMR (300 MHz, CDCl3) δ 1.36 (9H, s), 2.43 (3H, s), 2.86 (1H, m), 3.27 (2H, m), 3.50 (1H, m), 3.74 (1H, m), 4.07 (2H, m), 4.27 (1H, m), 5.04 (1H, m), 5.29 (2H, dd), 5.68 (1H, m), 6.30 (1H, m), 6.90 (2H, t), 7.22-7.37 (6H, m)

1. additionwas then added
2. customwhile being irradiated with microwaves
3. concentrationAfter concentration in a vacuum
4. customthe concentrate was purified by column chromatography
5. washeluting with a dichloromethane/methanol (35/1) eluent