反应 #1665766

ord-722db3be5b0d41d6b71325a73409ac56

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwere dropped in
  2. 2
    workup.STIRRINGthe reaction mixture was stirred into 3 1 of icewater
  3. 3
    萃取After extraction with methylene chloride
  4. 4
    其他to remove the acid
  5. 5
    workup.DISTILLATIONfrom the organic phase and distillation of the methylene chloride, distillation of the reaction

实验过程

100.8 g (1.2 mols) of diketene were added dropwise at -30°C to 0.5 1 of anhydrous hydrofluoric acid and a mixture of 0.6 mol of tetrahydronaphthalene and 0.6 mol of commercial grade dodecyl-benzene were dropped in. After stirring for 12 hours at room temperature, the reaction mixture was stirred into 3 1 of icewater. After extraction with methylene chloride, wahing with water to remove the acid from the organic phase and distillation of the methylene chloride, distillation of the reaction yielded 86 % of acetoacetyl-tetrahydronaphthalene boiling at 135°C under 0.5 torr and 77 g 40% of acetoacetyl-dodecyl-benzene boiling at 160°C under 0.5 torr as found by gas chromatographic determination of the fractions.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US03937737uspto-grants-1976_02