Reaction #331482

ord-eaec1fad2da5436f90a2a2760604dc88

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe mixture was refluxed for 6 hours
  2. 2
    FiltrationAfter the reaction product had been filtrated
  3. 3
    workup.ADDITIONsodium hydrogen carbonate was added to the filtrate
  4. 4
    Dryingthe organic layer was dried over magnesium sulfate

Procedure

The compound obtained in Step (11) was placed in a reaction vessel, and air in the vessel was replaced with nitrogen. After that, the compound was dissolved in dehydrated toluene (116 ml). Distilled DBU (6.0 ml, 40.1 mmol) was added to the solution, and the mixture was refluxed for 6 hours. After the reaction product had been filtrated, sodium hydrogen carbonate was added to the filtrate, and the organic layer was dried over magnesium sulfate, whereby 2,2-dimethyl-3a,7a-dihydrobenzo[1.3]dioxol was obtained. The compound was used in the next reaction without being further purified.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08658459B2uspto-grants-2014_02