반응 #339653

ord-fa171346fe3446d4b05bd4cecc1c2d29

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe resulting mixture was treated under μW at 95° C. for 20 min
  2. 2
    여과filtered through Celite®
  3. 3
    농축concentrated
  4. 4
    기타The resulting crude product was purified by chromatography (silica gel, 0-2% methanol in methylene chloride)
  5. 5
    기타to yield a white solid

실험 절차

To a solution of 5-cyano-6-(4-ethoxy-2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid (3,3-dimethyl-butyl)-amide (160 mg, 0.28 mmol) in methanol was added Zn (0.4 g) and NH4Cl (0.10 g). The resulting mixture was treated under μW at 95° C. for 20 min, filtered through Celite® and concentrated. The resulting crude product was purified by chromatography (silica gel, 0-2% methanol in methylene chloride) to yield a white solid that was converted to the HCl salt of the title compound by reacting with 1M HCl in diethyl ether.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07868022B2uspto-grants-2011_01