تفاعل #10410

معادلة التفاعل

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

المردود 67.0%

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

المردود 67.0%

المذيبات

N,N-dimethylformamide

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture is stirred at 25° C. for 18 hours
2. 2
   أخرىThe reaction is quenched with 1 mL of water
3. 3
   تركيزconcentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue is dissolved in chloroform
5. 5
   غسيلwashed with water, brine
6. 6
   تجفيفdried over magnesium sulfate
7. 7
   تركيزThe solution is concentrated
8. 8
   أخرىpurified via chromatography (SiO2, CHCl3)

الإجراء التجريبي

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+).

المصدر