2,2,2-Trifluoroethanol → 2,2,2-Trifluoroethyl trifluoroacetate

30 g (0.16 mole) of pyridinium trifluoroacetate in 355 g (3.55 mole) of 2,2,2-trifluoroethanol were introduced as an initial charge into a laboratory circulating reactor apparatus (one-liter four-necked flask fitted with KPG stirrer, a Prominent pump, and a 30 cm column packed with Raschig rings), and the initial charge was circulated at an internal temperature of 54° C. 134 g (1.01 mole) of trifluoroacetyl chloride were subsequently metered into the flask via an immersed inlet tube over a period of 100 minutes. After the trifluoroacetyl chloride addition was complete, the mixture was allowed to react for a further 10 minutes. Subsequent fractional distillation of the reaction mixture via a Vigreux column (temperature at the distillation head: from 54° to 56° C.) yielded 177.8 g of trifluoroethyl trifluoroacetate, corresponding to 89.8% of the theoretical yield. The trifluoroethanol/pyridinium salt mixture remaining in the reservoir flask can be used again for esterification with equal effectiveness.

1. additionan initial charge into a laboratory
2. customfitted with KPG stirrer
3. additioninitial charge
4. customwas circulated at an internal temperature of 54° C
5. customto react for a further 10 minutes
6. distillationSubsequent fractional distillation of the reaction mixture via a Vigreux column (temperature at the distillation head

ORD record

ord-be7ab524c7a74ff49ecf07a8293dd2e0

Source dataset

uspto-grants-1995_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05405991