반응 #78198

ord-046281170f08469dba7a019a60a28e30

반응 조건

온도
115°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated
  2. 2
    기타to obtain the crude product, which
  3. 3
    기타was purified by the silica gel column chromatography

실험 절차

18.0 g (46.4 mmol) of 3-[2-(t-butoxycarbonylamino)ethoxy]-4-iodobenzonitrile was dissolved in 200 ml of dimethylformamide (DMF). 13.3 g (92.8 mmol) of methyl 2-acetamidoacrylate, 2.82 g (9.28 mmol) of tris(2-methylphenyl)phosphine, 1.04 g (4.64 mmol) of palladium (II) acetate and 12.9 ml (92.8 mmol) of triethylamine were added to the obtained solution, and they were stirred at 115° C. for 4 hours. The solvent was evaporated to obtain the crude product, which was purified by the silica gel column chromatography to obtain the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710056B2uspto-grants-2004_03