Potassium Carbonate → HCID 15574961, compound

HRID 434636Notes

Reaction equation

HRID 434636 reaction equation
[CH3:1][C:2]([CH3:8])([CH2:6][OH:7])[C:3](=[O:5])[CH3:4].Cl[C:10]1[C:15]([Cl:16])=[CH:14][C:13]([C:17]([F:20])([F:19])[F:18])=[CH:12][N:11]=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH3:1][C:2]([CH3:8])([CH2:6][O:7][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([C:17]([F:20])([F:18])[F:19])=[CH:12][N:11]=1)[C:3](=[O:5])[CH3:4]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 1122342,3-Dichloro-5-(trifluoromethyl)pyridineHCID 111943184-Hydroxy-3,3-dimethylbutan-2-one

Product 1

HCID 15574961HCID 15574961, compoundYield 93.7%

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, 21.6 g of 2,3-dichloro-5-trifluoromethylpyridine and 15 g of anhydrous potassium carbonate were added thereto, and the system was gradually heated to 115° C. and stirred 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 26.7 g of oily 3,3-dimethyl-4-(3-chloro-5trifluoromethylpyridine-2-yloxy)butan-2-one.

Workup

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

Sources & evidence

ORD record
ord-6b1a3e9aa9dd4c6bbee09e9720c9302b
Source dataset
uspto-grants-1983_08
Patent number
US04399143

Reaction notes

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