反应详情

The procedure of Example 1 was followed using perfluoro-3-oxapentanesulfonyl fluoride (7.95 g, 25 mmol), potassium trimethylsilanolate (3.2 g, 25 mmol) and dry tetrahydrofuran (100 mL) while heating at reflux for 1.5 h. Potassium perfluoro-3-oxapentanesulfonate (3.79 g initially and 1.74 g by concentrating the filtrate under vacuum; total 5.53 g, 65% yield) was isolated as a white solid: 19F NMR (fluorotrichloromethane) δ -79.4 (m, CF2, 2F), -83.2 (s, CF3, 3F), -84.9 (m, CF2, 2F), -115.0 ppm (m, CF2, 2F); Positive ion Fast Atom Bombardment MS (Glycerol matrix, Cs⊕ ion bombardment) m/e 393, 747, 1101, 1455, 1809 for M+K⊕ to M5 +K⊕.

1. temperaturewhile heating
2. temperatureat reflux for 1.5 h
3. concentrationPotassium perfluoro-3-oxapentanesulfonate (3.79 g initially and 1.74 g by concentrating the filtrate under vacuum
4. customtotal 5.53 g, 65% yield) was isolated as a white solid