反应详情

温度

100 °C

To a stirred solution of 1-Boc-piperazine (18.9 g, 101.4 mmol) in 2-methoxyethanol (100 mL) was added 6-bromo-3-methyl-3H-pteridin-4-one (11.6 g, 48 mmol; see Example 16 (c) above) and the resulting suspension was heated for 3 hours at 100° C. The reaction was then cooled in an ice-water bath and the precipitate that formed was collected, washed with cold MeOH, and dried to afford 4-(3-methyl-4-oxo-3,4-dihydro-pteridin-6-yl)-piperazine-1-carboxylic acid tert-butyl ester as a yellow solid (15.2 g, 92%). 1H NMR (300 MHz, CDCl3) δ1.48 (s, 9H), 3.57-3.61 (m, 4H), 3.62 (s, 3H),3.78-3.82 (m, 4H), 8.07 (s, 1H), 8.56 (s, 1 H); 13C NMR (100 MHz, CDCl3) δ28.38, 34.42, 44.40, 80.38, 130.64, 137.93, 145.53, 147.04, 152.91, 154.61, 160.89.

1. temperatureThe reaction was then cooled in an ice-water bath
2. customthe precipitate that formed
3. customwas collected
4. washwashed with cold MeOH
5. customdried