反应详情

温度

60 °C

A mixture of N-(4-chlorobenzyl)-2-(chloromethyl)-3,4-dimethyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (85 mg, 0.21 mmol), 1-{3-[2-(2-methoxyethoxy)ethoxy]phenyl}-2-(methylamino)ethanol (Preparation 44) (85 mg, 0.32 mmol) and diisopropylethylamine (56 μL, 0.32 mmol) in dry DMF (4.4 mL) was heated to 60° C., becoming a solution. The reaction was stirred for 5 hours at that temperature. After cooling to room temperature, the solution was diluted with ice (6 g). The resulting milky suspension was stirred vigorously for 30 minutes, and then left standing overnight at room temp. The mixture was filtered, and the collected solid was washed with water and dried in vacuo, leaving a white solid. Recrystallization from acetonitrile/water (10 mL, 1:1, v/v, dissolved with warming acetonitrile, diluted with water and then cooled to 0° C. overnight) gave the title compound (107 mg) as a white solid.

1. temperatureAfter cooling to room temperature
2. stirringThe resulting milky suspension was stirred vigorously for 30 minutes
3. waitleft
4. waitstanding overnight at room temp
5. filtrationThe mixture was filtered
6. washthe collected solid was washed with water
7. customdried in vacuo
8. customleaving a white solid
9. customRecrystallization from acetonitrile/water (10 mL, 1:1, v/v
10. dissolutiondissolved with warming acetonitrile
11. additiondiluted with water
12. temperaturecooled to 0° C. overnight)