反応 #10410

反応方程式

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

収率 67.0%

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

収率 67.0%

溶媒

N,N-dimethylformamide

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture is stirred at 25° C. for 18 hours
2. 2
   その他The reaction is quenched with 1 mL of water
3. 3
   濃縮concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue is dissolved in chloroform
5. 5
   洗浄washed with water, brine
6. 6
   乾燥dried over magnesium sulfate
7. 7
   濃縮The solution is concentrated
8. 8
   その他purified via chromatography (SiO2, CHCl3)

実験手順

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+).

出典