反应 #1941

反应方程式

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

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

4-methylpiperazine

→

title compound

收率 96.9%

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

收率 96.9%

溶剂

methylene chloride

反应条件

后处理

1. 1
   浓缩The reaction mixture was concentrated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
3. 3
   洗涤The resultant solution was washed with 4 X 30 mL of water
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   过滤filtered
6. 6
   浓缩concentrated in vacuo

实验过程

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.

来源