Sodium Carbonate → 4-(2,2,3,3-Tetrafluoropropoxy)benzaldehyde

Participants

Reaction Conditions

Reaction Steps

138.2 g of potassium carbonate, 21.2 g of sodium carbonate, 198 g of tetrafluoropropanol and 124 g of 4-fluorobenzaldehyde are introduced at room temperature under argon protective gas and heated for 20 hours at 140° C. The boiling point of the reaction mixture is initially 125° C. As the reaction progresses, the internal temperature rises to 140° C. After 20 hours, the mixture is cooled to 25° C and filtered. This gives 229.6 g of filtrate containing 72% of 4-(2,2,3,3-tetrafluoropropoxy)benzaldehyde. The filter cake is washed 3 times using in each case 100 ml of toluene. Filtrate and toluene used for washing are collected separately. After 63.9 g of 2,2,3,3-tetrafluoropropanol have been distilled off from the filtrate, the distillation residue is combined with the toluene used for washing. After the toluene has been distilled off under atmospheric pressure, the residue is fractionated in vacuo at 3 mbar and a bottom temperature of up to 135° C. and a head temperature of 109° C. to 110° C. As the main fraction, 188.7 g of 4-(2,2,3,3-tetrafluoropropoxy)benzaldehyde with a purity (GC) of 98% to 99% are obtained.

Provenance & Evidence