反応 #1132453

反応方程式

PPVE

dimethyl 5-hydroxy-isophthalate

→

dimethyl 5-(1,1,2-trifluoro-2-(perfluoropropoxy)ethoxy)isophthalate

収率 85.1%

溶媒

THF

反応条件

後処理

1. 1
   その他In a nitrogen purged
2. 2
   その他dry box
3. 3
   その他equipped with a stirrer and addition funnel
4. 4
   その他to form a reaction mixture
5. 5
   その他the thus formed reaction mixture
6. 6
   温度was heated
7. 7
   その他The catalyst was then removed from the resulting mixture via filtration through a bed of silica gel
8. 8
   その他The filtrate thus produced
9. 9
   濃縮was concentrated under vacuum
10. 10
    その他a rotary evaporator
11. 11
    workup.DISTILLATIONfollowed by vacuum distillation

実験手順

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.

出典