반응 #1096246

ord-0be9011e355042fabde0abecf7eac40c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 48 hours
  2. 2
    기타The solvent was evaporated under a reduced pressure
  3. 3
    workup.DISSOLUTIONthe thus obtained residue was dissolved in ethyl acetate
  4. 4
    세척washed with water
  5. 5
    기타The solvent was again evaporated under a reduced pressure
  6. 6
    기타the residue was purified
  7. 7
    기타to obtain 1.90 g of the intended substance (yield 49.6%)

실험 절차

(2R,3S)-2-(2,4-Difluorophenyl)-3-methyl-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane (2.21 g, 8.8 mmol) and 1′,2′,3′,6′-tetrahydro-2,4′-bipyridine (7.47 g, 46.6 mmol) were dissolved in acetonitrile (100 ml), and lithium perchlorate trihydrate (7.48 g, 46.6 mmol) was added thereto and refluxed for 48 hours. The solvent was evaporated under a reduced pressure, and the thus obtained residue was dissolved in ethyl acetate and washed with water. The solvent was again evaporated under a reduced pressure, and the residue was purified using a silica gel column to obtain 1.90 g of the intended substance (yield 49.6%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07973056B2uspto-grants-2011_07