Trifluoroacetic acid → HCID 20030211, compound

HRID 1722039Notes

Reaction equation

HRID 1722039 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=O)[CH2:11][C:12](=[O:17])[C:13]([F:16])([F:15])[F:14])[C:5](O)=[CH:6][C:7]=1[Cl:8].FC(F)(F)C(O)=O>C(Cl)Cl>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]2[O:17][C:12]([C:13]([F:14])([F:15])[F:16])=[CH:11][CH:10]=[C:4]2[CH:3]=1

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 14773372HCID 14773372, compound

Product 1

HCID 20030211HCID 20030211, compoundYield 86%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of 4.62 g of crude product of the preceding Preparation, 4-(3,4-dichloro-6-hydroxyphenyl)-1,1,1-trifluoro-butan-2,4-dione (about 40% by NMR) and 4.6 ml trifluoroacetic acid in 27.6 ml methylene chloride was heated at reflux for 8 hours, then allowed to stand at 23° C. for 16 hours. The reaction was washed with 3×25 ml 1N sodium hydroxide and 25 ml brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give 2.0 g (86%) of product; m.p. 98°-101° C.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 8 hours
  3. washThe reaction was washed with 3×25 ml 1N sodium hydroxide and 25 ml brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-c56f97ac6b6e4704b7cd344c7cbd0e3e
Source dataset
uspto-grants-1989_08
Patent number
US04853410

Reaction notes

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