反应 #96019

反应方程式

N-(2-aminoethyl)acetoacetamide hydrobromide

Triethylamine

methacryloyl chloride

→

N-(2-acetoacetamidoethyl)-methacrylamide

收率 25.0%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   过滤The resulting solution was filtered
2. 2
   其他the solvent removed
3. 3
   workup.DISSOLUTIONthe residue dissolved in chloroform (500 ml)
4. 4
   洗涤The solution was then washed with 10% hydrochloric acid (200 ml)
5. 5
   干燥water (200 ml) and dried over anhydrous magnesium sulfate
6. 6
   其他The solvent was then removed
7. 7
   其他The residue was recrystallized from ethanol/ether (1:1)

实验过程

Crude N-(2-aminoethyl)acetoacetamide hydrobromide (50 g, 0.18 mole) was dissolved in N,N-dimethylformamide (500 ml). Triethylamine (78 g, 0.4 mole) and methacryloyl chloride (19 g, 0.18 mole) were added simultaneously at 0° C. The reaction solution was then stirred at 0° C. for 1 hour and at 20° C. for 20 hours. The resulting solution was filtered, the solvent removed, and the residue dissolved in chloroform (500 ml). The solution was then washed with 10% hydrochloric acid (200 ml), then water (200 ml) and dried over anhydrous magnesium sulfate. The solvent was then removed. The residue was recrystallized from ethanol/ether (1:1). The resulting compound had a m.p. of 86°-90° C. The yield was 25%.

来源