反应详情

温度

66 °C

In a nitrogen purged dry box, THF (500 mL) and dimethyl 5-hydroxy-isophthalate (42 g, 0.20 mol) were added to an oven-dried round bottom reaction flask equipped with a stirrer and addition funnel. Potassium carbonate catalyst (6.955 g, 0.0504 mol) was added via the addition funnel to form a reaction mixture. Subsequently PPVE (79.8 g, 0.30 mol) was added via the addition funnel and the thus formed reaction mixture was heated to reflux at 66° C. for 16 hours. The catalyst was then removed from the resulting mixture via filtration through a bed of silica gel. The filtrate thus produced was concentrated under vacuum using a rotary evaporator, followed by vacuum distillation to give 81.04 g (85.12% yield) of the desired dimethyl 5-(1,1,2-trifluoro-2-(perfluoropropoxy)ethoxy)isophthalate (F10-iso) collected as the distillate.

1. customIn a nitrogen purged
2. customdry box
3. customequipped with a stirrer and addition funnel
4. customto form a reaction mixture
5. customthe thus formed reaction mixture
6. temperaturewas heated
7. customThe catalyst was then removed from the resulting mixture via filtration through a bed of silica gel
8. customThe filtrate thus produced
9. concentrationwas concentrated under vacuum
10. customa rotary evaporator
11. distillationfollowed by vacuum distillation