反応 #331482

ord-eaec1fad2da5436f90a2a2760604dc88

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08658459B2uspto-grants-2014_02