反应详情

An amount of thionyl chloride of 8.99 g (0.08 mol) was introduced at 20-25° C. into a dry 50 ml round-bottomed flask under a nitrogen atmosphere. Ethyl 3-hydroxy-2-fluoropropionate (10.0 g, 0.07 mol) were subsequently metered in in 1 h and the mixture was subsequently stirred at ambient temperature for a further 2 h. An amount of toluene of 3.98 g (0.04 mol), together with 0.286 g of pyridine (5 mol %), were introduced into a second round-bottomed flask with an Anschutz head and the mixture was heated to 80° C., The mixture from the 1st round-bottomed flask was added dropwise to the preheated solution in 1 h at 75-85° C. Solvents were distilled off under reduced pressure and the residue was subsequently finely distilled at 120° C. and 10 mbar. 4.1 g of distillate were obtained as a colorless liquid.

1. customwere subsequently metered in in 1 h
2. temperaturethe mixture was heated to 80° C.
3. additionThe mixture from the 1st round-bottomed flask was added dropwise to the preheated solution in 1 h at 75-85° C
4. distillationSolvents were distilled off under reduced pressure
5. distillationthe residue was subsequently finely distilled at 120° C.
6. custom4.1 g of distillate were obtained as a colorless liquid