반응 #1941

반응 방정식

4-chloro-5-fluoro-2-(4-fluorobenzyl)-pyrimidine

4-Chloro-5-fluoro-2-(4-fluorobenzyl)-pyrimidine

4-methylpiperazine

→

title compound

수율 96.9%

5-Fluoro-2-(4-fluorobenzyl)-4-(4-methylpiperazin-1-yl)-pyrimidine

수율 96.9%

용매

methylene chloride

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
3. 3
   세척The resultant solution was washed with 4 X 30 mL of water
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

A mixture of 0.48 g (2 mmol) of 4-chloro-5-fluoro-2-(4-fluorobenzyl)-pyrimidine from Step 2 and 1.53 mL (14 mmol) of 4-methylpiperazine in 10 mL of methylene chloride was stirred at ambient temperature for 1.5 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in methylene chloride. The resultant solution was washed with 4 X 30 mL of water, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give 0.59 g (95% yield) of the title compound as an oil; 1H NMR (CDCl3) d 2.32 (s, 3H), 2.47 (t, 4H), 3.78 (t, 4H), 3.99 (s, 2H), 6.97 (m, 2H), 7.29 (m, 2H), 7.97 (d, 1H). The product was carried on to the next step without purification.

출처