반응 #471781

ord-bdc8d13bf6834d5f8a0217d1e8a14ec6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture is heated
  2. 2
    온도at reflux for several hours
  3. 3
    기타Upon completion of the reaction
  4. 4
    온도the mixture is cooled
  5. 5
    세척The organic layer is washed with water
  6. 6
    건조dried over anhydrous sodium sulfate
  7. 7
    농축concentrated

실험 절차

A solution of 26.03 g (0.100 mol) of 6-(4-methoxy-benzoyl)-7-oxa-bicyclo[4.2.0]octan-8-one in 200 ml of methylene chloride is added to 10.5 g (0.100 mol) of diethanolamine and 32 ml of N,N-diisopropylethylamine. The reaction mixture is heated at reflux for several hours and monitored by thin layer chromatography. Upon completion of the reaction, the mixture is cooled and poured into 1N hydrochloric acid solution. The organic layer is washed with water, dried over anhydrous sodium sulfate, and concentrated to give the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08367743B2uspto-grants-2013_02