反应详情

7-Iodo-2-methyl-5H-thiazolo[4,5-c]pyridin-4-one (880 mg, 3.01 mmol) was suspended in POCl3 (8.25 ml, 90.4 mmol) and refluxed for 4 hrs. The black reaction mixture was evaporated and poured as a dichloromethane solution in ice water. The aqueous layer was neutralized with solid NaHCO3 to pH 7 and extracted three times with dichloromethane. The combined organic extracts were dried with magnesium sulfate, filtered and evaporated. The crude product was purified by chromatography on silica gel (dichloromethane/methanol 100:0->95:5 gradient). The desired product was obtained as a light yellow solid (280 mg, 30%), MS: m/e=311.0 (M+H+).

1. temperaturerefluxed for 4 hrs
2. customThe black reaction mixture
3. customwas evaporated
4. additionpoured as a dichloromethane solution in ice water
5. extractionextracted three times with dichloromethane
6. dry with materialThe combined organic extracts were dried with magnesium sulfate
7. filtrationfiltered
8. customevaporated
9. customThe crude product was purified by chromatography on silica gel (dichloromethane/methanol 100:0->95:5 gradient)