반응 #2133675

ord-6fd862fbe7b14b27ab97e4c8382fd7bd

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was removed under reduced pressure
  2. 2
    여과the resulting solution was filtered
  3. 3
    기타The solvent was removed under reduced pressure
  4. 4
    기타the title compound was purified by column chromatography
  5. 5
    세척eluting with dichloromethane/methanol (90/10)

실험 절차

The title compound was prepared from 2-amino-7-biphenyl-2-yl-4-methyl-7,8-dihydro-6H-quinazolin-5-one oxime, compound 66, (100 mg, 0.290 mmol), 1-(3-chloro-propyl)-4-methyl-piperazine dihydrochloride (87 mg, 0.348 mmol) and sodium hydride (60% dispersion in oil) (52 mg, 1.31 mmol), following the same procedure used for 2-amino-7-(4-fluoro-biphenyl-2-yl)-4-methyl-7,8-dihydro-6H-quinazolin-5-one O-(3-dimethylamino-propyl)-oxime (compound 88), except after addition of water the solvent was removed under reduced pressure. The crude material was taken up in ethylacetate (20 ml) and the resulting solution was filtered. The solvent was removed under reduced pressure and the title compound was purified by column chromatography eluting with dichloromethane/methanol (90/10).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08592430B2uspto-grants-2013_11