Silicon tetrachloride → 3,5-Bis(trifluoromethyl)benzoyl chloride

Temperatur

40 °C

1040 g of 3,5-bis(trifluoromethyl)benzoyl fluoride and 24 g of aluminum chloride were initially introduced and heated to 40° C. With stirring, 224 g of silicon tetrachloride were added dropwise over 3 hours, where the temperature was controlled and did not exceed 45° C. The mixture was then stirred until the evolution of gas had stopped (2 hours). 30 g of zeolite X133 were then added, and the mixture was filtered. This gave 1000 g of a cloudy filtrate, which was admixed with 5 g of triphenylphosphine and distilled at 12 mbar over a 70 cm column. This gave 623 g (83.6% of theory) of 3,5-bis(trifluoromethyl)benzoyl chloride which passed over at 68° C. (bath temperature: 80° C.).

1. customdid not exceed 45° C
2. stirringThe mixture was then stirred until the evolution of gas
3. custom(2 hours)
4. filtrationthe mixture was filtered
5. distillationdistilled at 12 mbar over a 70 cm column
6. custompassed over at 68° C. (bath temperature: 80° C.)

ORD-Eintrag

ord-ecf16ddd89e74edf91f583c32b9d6690

Quelldatensatz

uspto-grants-2002_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06420601B2