反应详情

A mixture of N-(4-chlorobenzyl)-2-(chloromethyl)-3,4-dimethyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (100 mg, 0.25 mmol), 2-(methylamino)-1-pyrimidin-2-ylethanol (Preparation 61)(59 mg, 0.38 mmol) and diisopropylethylamine (67 μL, 0.38 mmol) in dry DMF (5 mL) was stirred for 72 hours at room temperature. The solution was diluted with water (7 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 (5 mL, dissolved with warming and then cooled to 0° C. overnight) gave the title compound (110 mg) as a white solid.

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