反応 #9474

ord-264de42745e6441b818c0fd73a192dd5

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to warm to ambient temperature
  2. 2
    その他A precipitate formed
  3. 3
    その他was isolated by filtration
  4. 4
    洗浄washed with water
  5. 5
    その他The crude solid was recrystallized from a mixture of isopropanol and acetonitrile

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091214B2uspto-grants-2006_08