반응 #159640

ord-faad08b707b74956ab0ae72080a6a1e1

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Solvents were evaporated in vacuo
  2. 2
    workup.ADDITIONThe obtained residue was diluted with water/1M HCl (5 ml/15 ml)
  3. 3
    추출extracted with ethyl acetate (3×30 ml)
  4. 4
    기타Collected fractions after solvent evaporation

실험 절차

To methyl 2-(2-benzylpyrrolidin-1-yl)-5-chloronicotinate (D74) (75 mg, 0.226 mmol) in a mixture 1,4-dioxane/water (3 ml/1 ml), lithium hydroxide monohydrate (14.3 mg, 0.34 mmol) was added and the resulting mixture was stirred at 150° C. under microwave irradiation for 10 min (2 cycles of 5 min each). Solvents were evaporated in vacuo. The obtained residue was diluted with water/1M HCl (5 ml/15 ml) and extracted with ethyl acetate (3×30 ml). Collected fractions after solvent evaporation afforded the title compound (D100) (70 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08828987B2uspto-grants-2014_09