반응 #527666

ord-53fbd4674cd04001afb9e599df1592d2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared in a similar manner to that
  2. 2
    기타to reach ambient temperature
  3. 3
    workup.ADDITIONwas added
  4. 4
    추출The product was extracted into ether
  5. 5
    기타the solvent then removed in vacuo

실험 절차

Sodium cyanoborohydride (10.7 g) was added at 0° C. to a mixture of 1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-methoxy-3,4-dihydroisoquinoline (26.7 g, prepared in a similar manner to that described above), acetic acid (185 ml) and methanol (95 ml) under nitrogen. The mixture was allowed to reach ambient temperature and was stirred for 22 hours. The mixture was poured onto water, and solid sodium hydroxide (150 g) in ice-water (500 ml) was added. The product was extracted into ether and the solvent then removed in vacuo to yield 1-[1-(2-chlorophenyl)cyclopropyl]-6-fluoro-7-methoxy-1,2,3,4-tetrahydroisoquinoline as a gum.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05519034uspto-grants-1996_05