反应 #1341

反应方程式

5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2-ene

trimethyl orthoacetate

isobutyric acid

→

5-bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene

反应条件

后处理

1. 1
   其他fitted with: nitrogen inlet/bubbler
2. 2
   温度The mixture was heated with agitation
3. 3
   温度to reflux
4. 4
   workup.DISTILLATIONdistillates collected until reaction mass temperature
5. 5
   其他the residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. @ 50 mmHg)

实验过程

5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2-ene (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).

来源