Реакция #10410

Уравнение реакции

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

Выход 67.0%

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

Выход 67.0%

Растворители

N,N-dimethylformamide

N,N-dimethylformamide

Условия реакции

Обработка

1. 1
   workup.STIRRINGthe mixture is stirred at 25° C. for 18 hours
2. 2
   ДругоеThe reaction is quenched with 1 mL of water
3. 3
   Концентрированиеconcentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue is dissolved in chloroform
5. 5
   Промывкаwashed with water, brine
6. 6
   Сушкаdried over magnesium sulfate
7. 7
   КонцентрированиеThe solution is concentrated
8. 8
   Другоеpurified via chromatography (SiO2, CHCl3)

Методика

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+).

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