反应详情

温度

60 °C

A mixture of N-(4-chlorobenzyl)-2-(chloromethyl)-4-methyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (100 mg, 0.26 mmol), 2-(methylamino)-1-pyrimidin-2-ylethanol (Preparation 23)(59 mg, 0.39 mmol) and diisopropylethylamine (67 μL, 0.38 mmol) in dry DMF (5 mL) was heated to 60° C., becoming a solution. The reaction was stirred for 7 hours at that temperature. After cooling to room temperature, the solution was diluted with water (10 mL). The resulting milky suspension was stirred vigorously for 30 minutes, and then left standing overnight in the refrigerator. The mixture was filtered, and the collected solid was washed with water and dried in vacuo, leaving a white solid. Recrystallization from acetonitrile/water (dissolved with warming 5 mL of acetonitrile, then cooled to 0° C. and then diluted with 2 mL of water, left overnight) gave the title compound (60 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 in the refrigerator
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. dissolutiondissolved
11. temperaturewith warming 5 mL of acetonitrile
12. temperaturecooled to 0° C.
13. additiondiluted with 2 mL of water
14. waitleft overnight)