반응 #84652

ord-69a23d5d36bf4cc69ee11cb718be1394

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was degassed with N2 for 5 mins
  2. 2
    온도The mixture was cooled to room temperature
  3. 3
    농축concentrated
  4. 4
    기타the residue was purified by silica gel column chromatography

실험 절차

A mixture of 2-chloro-6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazoline (0.95 g, 2.6 mmol), tert-butyl ((1S,2R)-2-aminocyclohexyl)carbamate (1.1 g, 5.14 mmol), and DBU (0.77 mL, 5.14 mmol) in acetonitrile (9 mL) was degassed with N2 for 5 mins and heated at 70° C. for 16 h. The mixture was cooled to room temperature, concentrated and the residue was purified by silica gel column chromatography to afford tert-butyl ((1S,2R)-2-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)cyclohexyl)carbamate (1.1 g, 81%). MS (ES+) C27H32Cl2N4O4 requires: 546, found: 547 [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434700B2uspto-grants-2016_09