반응 #9474

ord-264de42745e6441b818c0fd73a192dd5

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to warm to ambient temperature
  2. 2
    기타A precipitate formed
  3. 3
    기타was isolated by filtration
  4. 4
    세척washed with water
  5. 5
    기타The crude solid was recrystallized from a mixture of isopropanol and acetonitrile

실험 절차

Triethylamine (17.35 mL, 124 mmol) was added to a solution of 7-bromo-4-chloro-3-nitroquinoline (29.84 g, 104 mmol) in dichloromethane (253 mL), and the reaction was cooled to 0° C. 1-Amino-2-methylpropan-2-ol (10.17 g, 114 mmol) was added dropwise, and then the reaction was allowed to warm to ambient temperature and stirred overnight. A precipitate formed and was isolated by filtration and washed with water. The crude solid was recrystallized from a mixture of isopropanol and acetonitrile to provide 27.78 g of 1-(7-bromo-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08