反应 #96020

反应方程式

1-acetoacetylpiperazine hydrobromide

Triethylamine

methacryloyl chloride

→

4-acetoacetyl-1-methacryloylpiperazine

收率 56.0%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   过滤The reaction solution was filtered
2. 2
   其他the solvent was removed at low vacuum
3. 3
   workup.DISTILLATIONThe residue was distilled

实验过程

Crude 1-acetoacetylpiperazine hydrobromide (50 g, 0.2 mole) was dissolved in N,N-dimethylformamide (300 ml) with AranoxTM (50 mg) (available from U.S. Rubber Co.). Triethylamine (50 g, 0.5 mole) was added at 0° C., followed immediately by the dropwise addition of methacryloyl chloride (20.8 g, 0.2 mole) at 0° C. The reaction solution was then allowed to reach 20° C. over a 20 hour period. The reaction solution was filtered and the solvent was removed at low vacuum. The residue was distilled to give 4-acetoacetyl-1-methacryloylpiperazine (b.p.=110°-129° C./10-8μ) at a yield of 56%.

来源