反应详情

温度

25 °C

A mixture of 6-amino-2-butoxy-9-{3-[(3-piperidin-1-ylpropyl)amino]propyl}-7,9-dihydro-8H-purin-8-one dimaleate (20.0 g, 31.3 mmol), triethylamine (9.5 g, 94.1 mmol) and NMP (72 g) was stirred at 25° C. for 30 min. Sodium triacetoxyborohydride (11.3 g, 53.3 mmol) was added to the solution and stirred for 15 min. A solution of methyl (4-formylphenyl)acetate (8.4 g, 47.1 mmol) in NMP (10.3 g g) was added to the solution and the mixture stirred for 8 hr. Then NMP (41 g) was poured into the reaction solution and cooled to 5° C. To the solution was added cold water (200 g) dropwise and the mixture stirred. The reaction mixture was adjusted to pH9 by using 10% aqueous Na2CO3 and water (86 g) added. After stirring for 1 hr, the reaction mixture was filtered, the collecting solid washed with cooled water and dried to give the crude subtitle compound as a white solid. Yield 15.0 g, 84%.

1. stirringstirred for 15 min
2. stirringthe mixture stirred for 8 hr
3. temperaturecooled to 5° C
4. stirringthe mixture stirred
5. additionadded
6. stirringAfter stirring for 1 hr
7. filtrationthe reaction mixture was filtered
8. washthe collecting solid washed with cooled water
9. customdried