Calcium Carbonate → 2-Methoxycyclohexanone

HRID 1730440Notes

Reaction equation

HRID 1730440 reaction equation
Cl[CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[O:8].[C:9](=O)([O-])[O-:10].[Ca+2]>CO>[CH3:9][O:10][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[O:8]

Participants

4

Reactant 2

HCID 10112Calcium CarbonateHCID 132032-Chlorocyclohexanone

Product 1

HCID 1109982-MethoxycyclohexanoneYield 80%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

2-methoxycyclohexanone was prepared by dissolving 132 gm. 2-chlorocyclohexanone in 600 ml. of methanol in the presence of 50 gm. calcium carbonate and heating the suspension at 160° C. for 15-20 minutes. After removal of the methanol, the calcium chloride was precipitated by the addition of methylene chloride to the residual material. The calcium chloride was removed by filtration and the filtrate was distilled to yield an 80-85% yield of 2-methoxycyclohexanone.

Workup

  1. custom2-methoxycyclohexanone was prepared
  2. dissolutionby dissolving 132 gm
  3. customAfter removal of the methanol
  4. customthe calcium chloride was precipitated by the addition of methylene chloride to the residual material
  5. customThe calcium chloride was removed by filtration
  6. distillationthe filtrate was distilled

Sources & evidence

ORD record
ord-168f1daf4a6a48799feb493a4c4d4c4a
Source dataset
uspto-grants-1976_11
Patent number
US03992452

Reaction notes

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