Tetraglyme → HCID 131718529, Verbindung

In vacuo a mixture of cesium fluoride (1.2 g, 7.90 mmol), tetraglyme (2.4 g) and C3F7OCF(CF3)COF (5.22 g, 15.72 mmol) was stirred at -20° C. for 1 hour and at 0° C. also for 1 hour. Subsequently, the reaction was cooled to -196° C. and octafluoroisobutylene oxide (3.39 g, 15.70 mmol) was condensed into it. Next the reaction mixture was stirred at -22° C. for 17 hours and then at -17° C. for 24 hours. Following this operation the volatiles were removed and fractionated in vacuo through traps cooled to 0°, -23°, -47° and -196° C. The product, C3F7OCF(CF3)CF2OC(CF3)2COF, (4.15 g, 48% yield); VP 0° C. 0.5 mmHg, (following refractionation of the 0, -23 and -47 fractions) was collected in the -23° C. trap. The material was characterized by mass spectrometry in the form of its methyl ester, C3F7OCF(CF3)CF2OC(CF3)2CO2CH3, MS(70 eV) m/e (intensity,ion): 541 (65.8%, M-F), 491 (10.7%, M-CF3), 375 (72.5%, CF(CF3)CF 2 OC(CF3)2CO2CH3), 335 (60.6%, C3F7OCF(CF3)CF2), 275 (46.6%, CF2OC(CF3)2CO2CH3), 209 (67.3%, C(CF3)2CO2CH3).

1. temperatureSubsequently, the reaction was cooled to -196° C.
2. customcondensed into it
3. stirringNext the reaction mixture was stirred at -22° C. for 17 hours
4. waitat -17° C. for 24 hours
5. customwere removed
6. temperaturecooled to 0°, -23°, -47° and -196° C

ORD-Eintrag

ord-5b15d2e04c6a474a950bcad7bf5b1b8b

Quelldatensatz

uspto-grants-1994_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05326910