反应详情

温度

115 °C

2-Benzyl-4,5-dichloropyridazin-3(2H)-one (32.3 g, 127 mmol) was dissolved in hydriodic acid (223 mL) and the mixture was refluxed at 115° C. overnight. The mixture was poured into dichloromethane and 30% sodium thiosulphate (250 mL), and extracted with dichloromethane (3×250 mL). The combined organics were washed with 30% sodium thiosulphate several times (total 1 L), dried (sodium sulfate), and concentrated. Dichloromethane was added to the residue and the precipitate was collected by filtration to afford the title compound. 1H NMR (500 MHz, CD3SOCD3) δ 8.17 (s, 1H); 7.61 (s, 1H); 7.23-7.33 (m, 5H); 5.17 (s, 2H). LRMS (APCI) calc'd for (C11H10IN2O) [M+H]+, 313.0. found 313.0.

1. extractionextracted with dichloromethane (3×250 mL)
2. washThe combined organics were washed with 30% sodium thiosulphate several times (total 1 L)
3. dry with materialdried (sodium sulfate)
4. concentrationconcentrated
5. additionDichloromethane was added to the residue
6. filtrationthe precipitate was collected by filtration