Hydrochloric Acid → HCID 9795630, compound

HRID 322814Notes

Reaction equation

HRID 322814 reaction equation
[F:1][C:2]1[C:7]([C:8]([O:10]CC)=[O:9])=[C:6]([C:13]([O:15]CC)=[O:14])[C:5]([F:18])=[C:4]([F:19])[C:3]=1[CH:20](C(OCC)=O)[C:21]([O:23]CC)=[O:22].Cl>C(O)(=O)C>[F:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([C:13]([OH:15])=[O:14])[C:5]([F:18])=[C:4]([F:19])[C:3]=1[CH2:20][C:21]([OH:23])=[O:22]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 22011361HCID 22011361, compound

Product 1

HCID 9795630HCID 9795630, compoundYield 84.3%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To 50 g of diethyl 2-(2,5,6-trifluoro-3,4-bis(ethoxycarbonyl)phenyl)malonate were added 60 ml of conc. hydrochloric acid and 60 ml of acetic acid, and the mixture was refluxed overnight. The ethyl acetate in the reaction solution was distilled off under reduced pressure, and the solution was refluxed for 2 days. The acid in the reaction solution was distilled off, and hexane was added to the residue. The solid content was collected by filtration and dried to obtain 27 g of the title compound in crude form.

Workup

  1. temperaturethe mixture was refluxed overnight
  2. distillationThe ethyl acetate in the reaction solution was distilled off under reduced pressure
  3. temperaturethe solution was refluxed for 2 days
  4. distillationThe acid in the reaction solution was distilled off
  5. additionhexane was added to the residue
  6. filtrationThe solid content was collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-e1d2b1bb67d54c8ca1d1f523e3eae706
Source dataset
uspto-grants-2001_04
Patent number
US06211375B1

Reaction notes

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