반응 #67650

ord-5f4d3eb232c64b089e19cd6883476933

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was partitioned between water (40 mL) and ethyl acetate (3×40 mL)
  2. 2
    건조dried over Na2SO4
  3. 3
    여과filtered
  4. 4
    농축concentrated under reduced pressure

실험 절차

The product from Example 17B (0.35 g, 1.25 mmol) and the product from Example 17A (0.36 g, 1.29 mmol) in absolute ethanol (12 mL) were treated with sodium cyanoborohydride (94 mg, 1.50 mmol) and a catalytic amount of acetic acid. The resulting mixture was stirred at ambient temperature overnight. The mixture was partitioned between water (40 mL) and ethyl acetate (3×40 mL). The organic layers were combined, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel (hexanes:ethyl acetate, 1:1) to provide the title compound (0.15 g, 22%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524753B2uspto-grants-2013_09