反応 #10417

反応方程式

NH4Cl

1-cyclopropyl-3-(3-methoxy-2,4,5-trifluorobenzoyl)urea

sodium hydride

→

title compound

1-Cyclopropyl-6,7-difluoro-8-methoxy-1H-quinazoline-2,4-dione

溶媒

tetrahydrofuran

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度heated
2. 2
   温度at reflux for 16 hours
3. 3
   温度The mixture is cooled
4. 4
   抽出extracted with dichloromethane
5. 5
   洗浄The organic layer is then washed with brine
6. 6
   乾燥dried over Na2SO4
7. 7
   濃縮concentrated under reduced pressure

実験手順

A solution of 1-cyclopropyl-3-(3-methoxy-2,4,5-trifluorobenzoyl)urea (Example 27b, 0.94 g, 3.26 mmol) in tetrahydrofuran (20 mL) and N,N-dimethylformamide (5 mL) is treated with sodium hydride (0.275 g, 6.8 mmol, 60% in mineral oil dispersion) and heated at reflux for 16 hours. The mixture is cooled, treated with saturated NH4Cl and extracted with dichloromethane. The organic layer is then washed with brine, dried over Na2SO4 and concentrated under reduced pressure. Flash column chromatography (1:3 ethyl acetate/hexanes) afforded the title compound. MS (EI, M+1) m/z 269.

出典