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 (195 mg, 0.49 mmol), (1R)-2-(methylamino)-1-pyrimidin-2-ylethanol (Preparation 104, 168 mg, 0.74 mmol) and diisopropylethylamine (430 μL, 2.5 mmol) in dry DME (10 mL) was heated to 60° C., becoming a solution. The reaction was stirred overnight at that temperature. After cooling to room temperature, the solution was diluted with ice water (30 mL). 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 (30 mL, dissolved with warming and then cooled to 0° C. overnight) gave the title compound (105 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 (30 mL
10. dissolutiondissolved
11. temperaturewith warming
12. temperaturecooled to 0° C. overnight)