반응 #735826

ord-b7106683cbda4aa2b9b35f7c7db631bb

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 24 hours
  2. 2
    기타evaporated in vacuo
  3. 3
    workup.DISSOLUTIONdissolved in chloroform
  4. 4
    추출extracted with dilute sodium bicarbonate solution
  5. 5
    세척The organic phase was washed with water
  6. 6
    기타dried
  7. 7
    여과filtered
  8. 8
    기타evaporated in vacuo
  9. 9
    기타The evaporation residue was purified by column chromatography on silica gel (toluene/acetone=5:1)

실험 절차

A mixture of 2 gm (5.46 m mol) of 4-[(1-(2-piperidinophenyl)-ethyl)-aminocarbonylmethyl]-benzoic acid, 0.53 gm of methanol, 0.38 ml of conc. sulfuric acid, and 1.65 ml of 1,2-dichloro-ethane was refluxed for 24 hours, then evaporated in vacuo, dissolved in chloroform, and extracted with dilute sodium bicarbonate solution. The organic phase was washed with water, dried, filtered, and evaporated in vacuo. The evaporation residue was purified by column chromatography on silica gel (toluene/acetone=5:1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04735959uspto-grants-1988_04