Reaction #352846

ord-ea6d5fd77e3b46ab88a2f2da7ccd038e

Reaction equation

O=C1OC(=O)c2c(F)c(F)c(F)c(F)c21
tetrafluorophthalic anhydride
CCCCCCCCN(CCCCCCCC)CCCCCCCC
tri-n-octylamine
CO
methanol
COC(=O)c1cc(F)c(F)c(F)c1F
3,4,5,6-tetrafluorobenzoic acid methyl ester
Yield 92.4%

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherInto a 100 ml glass reactor equipped with a reflux condenser and a stirrer
  2. 2
    OtherThen, the mixture was reacted at 140° C. for 4 hours
  3. 3
    OtherAfter completion of the reaction
  4. 4
    Otherthe reaction mixture was separated by distillation

Procedure

Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer, 20 g (0.091 mol) of the tetrafluorophthalic anhydride prepared in Example 3 and 32.2 g (0.091 mol) of tri-n-octylamine were charged and 3.5 g (0.109 mol) of methanol was dropwise added thereto. Then, the mixture was reacted at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 17.5 g of 3,4,5,6-tetrafluorobenzoic acid methyl ester. The yield was 92.3%.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05648504uspto-grants-1997_07