Reacción #10410

Ecuación de reacción

3-dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione

3-Dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione

sodium hydride

Bromomethylcyclopropane

→

title compound

Rendimiento 67.0%

3-Dibenzylamino-6,7-difluoro-1-cyclopropylmethyl-1H-quinazoline 2,4-dione

Rendimiento 67.0%

Disolventes

N,N-dimethylformamide

N,N-dimethylformamide

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGthe mixture is stirred at 25° C. for 18 hours
2. 2
   OtroThe reaction is quenched with 1 mL of water
3. 3
   Concentraciónconcentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue is dissolved in chloroform
5. 5
   Lavadowashed with water, brine
6. 6
   Secadodried over magnesium sulfate
7. 7
   ConcentraciónThe solution is concentrated
8. 8
   Otropurified via chromatography (SiO2, CHCl3)

Procedimiento

A solution of 3-dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione (Example 16) (0.43 g, 1.1 mmol) in 10 mL of N,N-dimethylformamide is added to a suspension of sodium hydride (0.05 g, 1.3 mmol) in 10 mL of N,N-dimethylformamide and stirred for 30 minutes. Bromomethylcyclopropane (0.16 mL, 1.6 mmol) is added, and the mixture is stirred at 25° C. for 18 hours. The reaction is quenched with 1 mL of water and concentrated in vacuo. The residue is dissolved in chloroform, washed with water, brine, and dried over magnesium sulfate. The solution is concentrated and purified via chromatography (SiO2, CHCl3) to give 0.33 g of the title compound as a solid. MS CI: m/z 448 (MH+).

Fuente