반응 #53611

ord-bef4abc45ff44e46be142e66008f7e76

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The catalyst was filtered off
  2. 2
    농축the filtrate was concentrated under reduced pressure
  3. 3
    기타The residue obtained
  4. 4
    기타was chromatographed on aluminum oxide in chloroform

실험 절차

Compound (29) 609 mg was dissolved in tetrahydrofuran 20 ml. 20% Palladium(II)hydroxide 200 mg was added. A mixture was stirred in a hydrogen atomosphere for 22 h. The catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in chloroform to give the titled compound (31) as pale brown crystals, 337 mg. Yield 86%. Furthermore, this was recrystallized from methanol-isopropanol to give the titled compound (31) as pale brown crystals, m.p. 202-203° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06858640B2uspto-grants-2005_02