反応 #9598
ord-9312b9100a3448fd880c4a1e4f95c690
反応方程式
溶媒
反応条件
温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1濃縮concentrated under reduced pressure
- 2workup.DISSOLUTIONThe residue was dissolved in water
- 3その他was isolated by filtration
- 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.