Acetic Acid → HCID 76539464, compound

HRID 1669790Notes

Reaction equation

HRID 1669790 reaction equation
O=[C:2]([CH3:13])[CH2:3][C:4]([O:6][CH:7]([CH3:12])[C:8]([F:11])([F:10])[F:9])=[O:5].C([O-])(=O)C.[NH4+:18].C(O)(=O)C>O>[NH2:18][C:2]([CH3:13])=[CH:3][C:4]([O:6][CH:7]([CH3:12])[C:8]([F:11])([F:10])[F:9])=[O:5]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 517165Ammonium AcetateHCID 57438897HCID 57438897, compound

Product 1

HCID 76539464HCID 76539464, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2.4 g (12 mmol) of 2,2,2-trifluoro-1-methylethyl 3-oxobutanoate are heated with 1.8 g (24.6 mmol) of ammonium acetate and 0.6 g (11 mmol) of acetic acid with the addition of molecular sieves at 110° C. for 5 h. After cooling to room temperature, the reaction mixture is mixed with water and extracted with ethyl acetate. Washing of the organic phase with water and saturated sodium chloride solution is followed by drying over magnesium sulfate. After filtration, the solvent is removed in vacuo. The resulting crude product (1.5 g, 77% purity, 77% of theory) is employed without further purification in the next stage.

Workup

  1. extractionextracted with ethyl acetate
  2. washWashing of the organic phase with water and saturated sodium chloride solution
  3. dry with materialby drying over magnesium sulfate
  4. filtrationAfter filtration
  5. customthe solvent is removed in vacuo
  6. customThe resulting crude product (1.5 g, 77% purity, 77% of theory) is employed without further purification in the next stage

Sources & evidence

ORD record
ord-d403b23bd4954b928d5c3b7a449ed7b4
Source dataset
uspto-grants-2011_08
Patent number
US07989633B2

Reaction notes

Loading…