反应详情

温度

140 °C

Chlorosulfonic acid (4.10 mL, 62.6 mmol) was slowly added to quinazolin-4-ol (1.09 g, 0.26 mmol). The resulting mixture was heated to 140° C. and stirred for 3 hours at the same temperature. After cooling to room temperature, the reaction mixture was poured into crushed ice. The mixture was extracted with DCM (100 mL×3), the combined organic layers were dried over Na2SO4, filtered, and the filtrate was concentrated in vacuo. The residue was purified via flash chromatography (5% PE: Ethyl Acetate) to give 370 mg of 4-hydroxyquinazoline-8-sulfonyl chloride. 1H NMR (400 MHz, DMSO-d6) δ: 7.76 (t, J=7.79 Hz, 1H) 8.26 (ddd, J=9.67, 7.92, 1.48 Hz, 2H) 9.02 (s, 1H). LC-MS: m/z 245.7 (M+H)+

1. temperatureAfter cooling to room temperature
2. additionthe reaction mixture was poured
3. custominto crushed ice
4. extractionThe mixture was extracted with DCM (100 mL×3)
5. dry with materialthe combined organic layers were dried over Na2SO4
6. filtrationfiltered
7. concentrationthe filtrate was concentrated in vacuo
8. customThe residue was purified via flash chromatography (5% PE: Ethyl Acetate)