Potassium Carbonate → HCID 13200578, compound

HRID 434637Notes

Reaction equation

HRID 434637 reaction equation
[CH3:1][C:2]([CH3:8])([CH2:6][OH:7])[C:3](=[O:5])[CH3:4].[F:9][C:10]([F:19])([F:18])[C:11]1[CH:12]=[N:13][C:14](Cl)=[CH:15][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH3:1][C:2]([CH3:8])([CH2:6][O:7][C:14]1[CH:15]=[CH:16][C:11]([C:10]([F:19])([F:18])[F:9])=[CH:12][N:13]=1)[C:3](=[O:5])[CH3:4]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 923422-Chloro-5-(trifluoromethyl)pyridineHCID 111943184-Hydroxy-3,3-dimethylbutan-2-one

Product 1

HCID 13200578HCID 13200578, compoundYield 98.5%

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Conditions

Temperature
115 °C

Procedure

3,3-Dimethyl-4-hydroxybutan-2-one (11.2 g) was dissolved in 50 ml of dimethyl sulfoxide, and nitrogen gas was passed therethrough for 20 minutes. Then, 18.2 g of 3-trifluoromethyl-6-chloropyridine and 15 g of anhydrous potassium carbonate were added thereto, and the solution was gradually heated to 115° C. and reacted under stirring for 4 hours at that temperature. After completion of the reaction, the product was put into ice water, extracted with methylene chloride, washed with water and dried over Glauber's salt. The solvent was distilled off to give 24.8 g of oily 3,3-dimethyl-4-(5-trifluoromethylpyridine-2-yloxy)butan-2-one.

Workup

  1. customreacted
  2. customAfter completion of the reaction
  3. extractionextracted with methylene chloride
  4. washwashed with water
  5. dry with materialdried over Glauber's salt
  6. distillationThe solvent was distilled off

Sources & evidence

ORD record
ord-986b7dfd4b024604b084e961e63ab860
Source dataset
uspto-grants-1983_08
Patent number
US04399143

Reaction notes

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