تفاعل #64707

ord-9a96245cefaa4e4aac5f8161d0bf5ca1

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.STIRRINGThe resulting mixture was stirred for 1 hour
  3. 3
    استخلاصextracted with methylene chloride
  4. 4
    أخرىAfter drying the organic layer
  5. 5
    أخرىthe solvent was evaporated under reduced pressure
  6. 6
    غسيلeluted with hexane-ethyl acetate (6:1)

الإجراء التجريبي

A mixture of 2-phenoxybenzoyl chloride (1.09 g) and methyl isocyanide (383 mg) was stirred at 50° C. for 3 hours. Then, the mixture was diluted with acetone (10 ml), and water (2 ml) and calcium carbonate (500 mg) were added. The resulting mixture was stirred for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. After drying the organic layer, the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (6:1) to obtain the title compound as crystals (1.04 g, Yield: 87.1%), mp: 94°-95° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05414122uspto-grants-1995_05