반응 #325419

ord-7e1d6d8076e343e881b81f801cb65135

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux for 6 hr
  2. 2
    기타the solvent was removed in vacuo
  3. 3
    workup.ADDITIONThe residue was diluted with water
  4. 4
    추출extracted with EtOAc (300 mL×3)
  5. 5
    건조the organic layer was dried with Na2SO4
  6. 6
    농축concentrated
  7. 7
    기타purified by column chromatography

실험 절차

A solution of 4-[1-(2-carbamoyl-phenylcarbamoyl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester (20 g, 0.05 mmol, crude from the last step) and MeONa (10 g, 0.19 mol) in MeOH (500 mL) was heated to reflux for 6 hr and the solvent was removed in vacuo. The residue was diluted with water and extracted with EtOAc (300 mL×3), the organic layer was dried with Na2SO4, concentrated and purified by column chromatography to afford the product (2 g, 5%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08642609B2uspto-grants-2014_02