Acetic Acid → HCID 20163295, compound

HRID 246894Notes

Reaction equation

HRID 246894 reaction equation
[CH3:1][C:2]1([C:10](=[O:12])[CH3:11])[CH:7]([CH3:8])[CH2:6][C:5]([CH3:9])=[CH:4][CH2:3]1.[C:13](O)(=O)C>>[CH3:1][C:2]1([C:10]([OH:12])([CH3:13])[CH3:11])[CH:7]([CH3:8])[CH2:6][C:5]([CH3:9])=[CH:4][CH2:3]1

Participants

3

Reactant 2

HCID 176Acetic AcidHCID 201632901-(1,4,6-Trimethylcyclohex-3-en-1-yl)ethan-1-one

Product 1

HCID 20163295HCID 20163295, compound

Procedure

0.4 moles (66.4 g) 1-(1,4,6-trimethylcyclohex-3-en-1-yl)-ethan-1-one (as per Example 1) was then added dosewise at 70° C. to the reaction mixture according to (a). Then stirring was continued for another hour at 70° C. The reaction mixture was then cooled, poured on 300 g ice, and the precipitated magnesium salt was dissolved with 30 ml glacial acetic acid. Finally the phases were separated, the organic phase neutralized with sodium bicarbonate solution, the solvent drawn off and the residue subjected to fractional distillation. 30 g of the desired end product were obtained, corresponding to 40% of the theoretical amount.

Workup

  1. waitwas continued for another hour at 70° C
  2. temperatureThe reaction mixture was then cooled
  3. customFinally the phases were separated
  4. distillationthe residue subjected to fractional distillation
  5. custom30 g of the desired end product were obtained, corresponding to 40% of the theoretical amount

Sources & evidence

ORD record
ord-a48684bc17e34fb4849ed55d95858785
Source dataset
uspto-grants-1987_11
Patent number
US04704477

Reaction notes

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