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 (25 mg, 0.063 mmol), 1-(methylamino)methyl(phenyl)phosphinic acid (R. Tyka, Synthesis 1984, 218) (24 mg, 0.0.13 mmol) and potassium carbonate (35 mg, 0.25 mmol) in dry DMF (1.0 mL) and water (0.25 mL) was stirred at 60° C. for 30 minutes, going to a solution. HPLC analysis indicated reaction was complete. The solvent was removed in vacuo, and the resulting white solid was washed with methylene chloride. The solid was dissolved in water (5 mL) and brought to pH 7 with 1.0 M aqueous HCl. After standing in a 0° C. refrigerator overnight, the mixture was filtered, and the collected solid was washed with cold water. Drying in vacuo left the title compound as a white powder (23 mg).

1. customreaction
2. customThe solvent was removed in vacuo
3. washthe resulting white solid was washed with methylene chloride
4. dissolutionThe solid was dissolved in water (5 mL)
5. customAfter standing in a 0° C.
6. customrefrigerator overnight
7. filtrationthe mixture was filtered
8. washthe collected solid was washed with cold water
9. customDrying in vacuo
10. waitleft the title compound as a white powder (23 mg)