反应详情

To 2-iodo-4-oxo-4,5-dihydro-thieno[3,2-c]pyridine-7-carbonitrile 25 (7.75 g, 25.6 mmol) was added POCl3 (90 mL). The reaction was stirred under reflux overnight. POCl3 was removed by rotary evaporation followed by suspension of solids in H2O (500 mL) and filtration. The solids were washed with copious amounts of H2O, saturated bicarbonate solution, and washed further with H2O to provide upon drying 7.52 g of 26. 1H NMR (400 MHz, d6-DMSO) δ 8.82 (s, 1H), 8.06 (s, 1H).

1. temperatureunder reflux overnight
2. customPOCl3 was removed by rotary evaporation
3. additionfollowed by suspension of solids in H2O (500 mL)
4. filtrationfiltration
5. washThe solids were washed with copious amounts of H2O, saturated bicarbonate solution
6. washwashed further with H2O
7. customto provide
8. dry with materialupon drying 7.52 g of 26