반응 #10411

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

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

sodium hydride

Ethyl iodide

→

title compound

수율 73.3%

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

수율 73.3%

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred at 25° C. for 18 hours
2. 2
   기타The reaction is quenched with 1 mL of water
3. 3
   농축concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue is dissolved in chloroform
5. 5
   세척washed with water, brine
6. 6
   건조dried over magnesium sulfate
7. 7
   농축The solution is concentrated
8. 8
   기타purified via chromatography (SiO2, CHCl3)

실험 절차

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. Ethyl iodide (0.13 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 0.34 g of the title compound as a solid, mp 133–135° C., MS CI, m/z 422 (MH+).

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