反应详情

温度

81.5 °C

Add 6-fluoro-2-methyl-4,9-dihydro-3-thia-4,9-diaza-benzo[f]azulen-10-one (65.2 g, 0.263 mol) and 2,4-Bis-(4-methoxy-phenyl)-[1,3,2,4]dithiadiphosphetane 2,4-disulfide (Lawesson's Reagent, 63.7 g, 0.157 mol) to 1,2-dichloroethane (DCE, 3500 mL) with stirring. Heat to gentle reflux (80-83° C.) for 30 minutes, and then allow cooling to ambient temperature. Filter the product and rinse with DCE. Dry at 50-60° C. to give 61.9 (89%) the title compound: 1H NMR (400 MHz, DMSO-d6) δ 10.98 (bs, 1H), 8.87 (bs, 1H), 7.00 (m, 1H), 6.88 (s, 1H), 6.78(m, 1H), 6.56 (m, 1H), 2.22 (s, 3H). HRMS (ES) exact mass M+H calcd for C12H9FN2S2 265.0269; found 265.0276.

1. temperatureHeat
2. temperatureallow cooling to ambient temperature
3. filtrationFilter the product
4. washrinse with DCE
5. customDry at 50-60° C.