반응 #78342

ord-f98a0dfd4ce943b2aa9e96003bff4d61

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The catalyst is filtered off
  2. 2
    농축the filtrate is concentrated under vacuum
  3. 3
    기타The residue is chromatographed on silica H
  4. 4
    기타The product obtained
  5. 5
    기타the precipitate formed
  6. 6
    여과is filtered off

실험 절차

A mixture of 2.3 g of the compound obtained in EXAMPLE 8 and 0.3 g of Raney® nickel in 100 ml of EtOH is hydrogenated for 72 hours at RT and at atmospheric pressure. The catalyst is filtered off and the filtrate is concentrated under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (85/15; v/v) as the eluent. The product obtained is taken up with ethereal hydrogen chloride and the precipitate formed is filtered off to give 1.08 g of the expected product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710042B2uspto-grants-2004_03