반응 #55019

ord-37c6f292c96845a9b52d30991246307e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    온도the whole is heated
  3. 3
    온도to reflux
  4. 4
    온도at reflux temperature for 3h
  5. 5
    온도The reaction mixture is cooled
  6. 6
    여과filtered
  7. 7
    세척The benzene-phase is washed with water
  8. 8
    기타After evaporation
  9. 9
    기타an oily residue is obtained
  10. 10
    기타on triturating in 1,1'-oxybisethane

실험 절차

to a stirred solution of 8 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate in 4 parts of pyridine and 80 parts of benzene are added dropwise 7.7 parts of benzeneacetyl chloride in 40 parts of benzene. After the addition is complete, the whole is heated to reflux and stirred at reflux temperature for 3h. 45. The reaction mixture is cooled and filtered. The benzene-phase is washed with water and then with sodium hydrogen carbonate solution and with water. After evaporation, an oily residue is obtained, which solidifies on triturating in 1,1'-oxybisethane, to yield 5 parts of ethyl 4-[N-(2,6-dimethylphenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 106° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04151286uspto-grants-1979_04