反応 #9598

ord-9312b9100a3448fd880c4a1e4f95c690

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water
  3. 3
    その他was isolated by filtration
  4. 4
    その他air-dried for 48 hours

実験手順

To a stirred solution of 1-[2-(3-amino-7-bromoquinolin-4-ylamino)ethyl]-3-(2-methylethyl)urea (27.2 g, 0.0743 mol) in 600 mL pyridine was slowly added ethoxyacetyl chloride (1.1 equivalents). After 1.5 hours the mixture was yellow and turbid. The reaction mixture was then heated at 80° C. for 12 hours and then concentrated under reduced pressure. The residue was dissolved in water and saturated aqueous potassium carbonate and stirred vigorously for three hours. A precipitate was present, was isolated by filtration, and air-dried for 48 hours to provide 32 g of 1-[2-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]-3-(2-methylethyl)urea.

出典

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