Phosphoric Acid → HCID 56960321, compound
Reaction equation
P(=O)(O)(O)O.[CH3:6][C:7]1[CH2:12][CH2:11][C:10]([CH3:15])([CH:13]=[CH2:14])[CH2:9][CH:8]=1>C1(C)C=CC=CC=1>[CH3:6][C:7]1[CH:12]2[CH2:11][C:10]([CH3:15])([CH2:9][CH:8]=1)[CH2:13][CH2:14]2Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Phosphoric acid (H3PO4, 145 g, 1.48 mol) was added to a solution of 1,4-dimethyl-4-vinyl-cyclohexene (403 g, 2.96 mol, commercially available from Evonik Industries) in toluene (500 mL) and refluxed for 6 hours. The reaction mixture was subsequently quenched with a solution of sodium hydroxide (NaOH). The organic layer was separated, dried over sodium sulfate (Na2SO4), and fractionated to provide 2,5-dimethyl-bicyclo[3.2.1]oct-2-ene (280 g) having a boiling point of 87° C. at a pressure of 27 mmHg.
Workup
- customThe reaction mixture was subsequently quenched with a solution of sodium hydroxide (NaOH)
- customThe organic layer was separated
- dry with materialdried over sodium sulfate (Na2SO4)
Sources & evidence
- ORD record
- ord-282057bf50014d7a8876940cf3ee364c
- Source dataset
- uspto-grants-2013_01
- Patent number
- US08357358B2
Reaction notes
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