تفاعل #10417

معادلة التفاعل

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

المذيبات

tetrahydrofuran

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةat reflux for 16 hours
3. 3
   درجة الحرارةThe mixture is cooled
4. 4
   استخلاصextracted with dichloromethane
5. 5
   غسيلThe organic layer is then washed with brine
6. 6
   تجفيفdried over Na2SO4
7. 7
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

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.

المصدر