反应详情

温度

100 °C

Process step c): 185.3 g (1.25 mol) of triethyl orthoformate were initially charged in a stirred vessel, the pressure in the vessel was reduced to 500 mbar and the triethyl orthoformate was heated to 100° C. 177.5 g (0.25 mol-100% conversion in process steps a) and b) assumed) of ethyl 4,4-difluoroacetoacetate (in the form of a suspension coming from process step b)) were added at 98° C. to 105° C. within 2 hours. Thereafter, the reaction mixture was stirred at 100° C. for further 3.5 hours. Within this post reaction time the pressure was further reduced to 300 mbar. During the whole reaction time low boiling compounds were removed by distillation under reduced pressure. The resulting suspension (191 g) comprised 16.7% (w/w) of the desired product (GC analysis, quantification with internal standard). The yield, based on ethyl difluoroacetate used, was 57.3%.

1. additionwere added at 98° C. to 105° C. within 2 hours
2. customWithin this post reaction time the pressure
3. customDuring the whole reaction time low boiling compounds were removed by distillation under reduced pressure