Potassium Iodide → HCID 18359436, compound

HRID 428809Notes

Reaction equation

HRID 428809 reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=[O:11])[CH3:10])=[CH:4][CH:3]=1.Cl[CH2:13][Si:14]([CH3:23])([CH3:22])[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CS(C)=O.C(OCC)C>[CH3:13][Si:14]([CH2:23][O:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9](=[O:11])[CH3:10])=[CH:6][CH:7]=1)([CH3:22])[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1

Participants

7

Reactant 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 70192744-HydroxyphenylacetoneHCID 13392358(Chloromethyl)(4-fluorophenyl)dimethylsilane

Product 1

HCID 18359436HCID 18359436, compound

Reagents, catalysts & solvents 2

HCID 679Dimethyl SulfoxideSolventHCID 3283Diethyl EtherSolvent

Procedure

30 g of 1-(4-hydroxyphenyl)-propan-2-one and 45.5 g of chloromethyl-dimethyl-(4-fluorophenyl)-silane in 400 ml of dimethyl sulfoxide are stirred with 42 g of potassium carbonate and 2 g of potassium iodide for 12 hours at 70° C. The reaction mixture is poured into 1.6 liters of ice water and 500 ml of diethyl ether are added; the ether phase is extracted by washing several times with water and saturated sodium chloride solution and dried over sodium sulfate; the solvent is evaporated off. Distillation at 150° C. (0.01 mbar) yields the title product.

Workup

  1. additionare added
  2. extractionthe ether phase is extracted
  3. washby washing several times with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customthe solvent is evaporated off
  6. distillationDistillation at 150° C. (0.01 mbar)

Sources & evidence

ORD record
ord-f92490fc3a8945b38c23a47081af8dc9
Source dataset
uspto-grants-2001_11
Patent number
US06313344B1

Reaction notes

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