Isobutyric Acid → HCID 19936152, compound

Temperature

111 °C

5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2ene (10.0 g), trimethyl orthoacetate (48.0 g) and isobutyric acid (0.29 g) were charged to a round-bottomed flask fitted with: nitrogen inlet/bubbler, thermometer and Dean and Stark received packed with 5A molecular seives. The mixture was heated with agitation to reflux and distillates collected until reaction mass temperature increased to 111° C. (ca. 1 hr). Once the reaction was complete, the residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. ≃50 mmHg) to give the product, 5-bromo-5-chloro-4-1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene, as an orange oil (10.9 g, 85% yield).

1. customfitted with: nitrogen inlet/bubbler
2. temperatureThe mixture was heated with agitation
3. temperatureto reflux
4. distillationdistillates collected until reaction mass temperature
5. customthe residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. ≃50 mmHg)

ORD record

ord-fcee9aa287524ea18dc987ee5bcad3e9

Source dataset

uspto-grants-1996_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05527972