反应 #1810841
ord-0ffa5dac74b64c51b39a39b1efa6292b
反应方程式
1-Cyclobutyl-2-methyl-4-acetylimidazole
DMF
DMA
→
title compound
收率 47.0%
5-(3-Dimethylaminoprop-2-enoyl)-1-cyclobutyl-2-methylimidazole
收率 47.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度at reflux, under an atmosphere of nitrogen, for 54 hours
- 2其他crystallised
- 3过滤The solid product was collected by filtration
- 4洗涤washed with DMF
- 5干燥DMA and then ether and dried under vacuum at 40° C.
实验过程
1-Cyclobutyl-2-methyl-4-acetylimidazole (Method 3; 2.52 g, 14.1 mmol) was dissolved in DMF.DMA (75 mL) and the mixture heated at reflux, under an atmosphere of nitrogen, for 54 hours. The reaction mixture was allowed to cool to ambient temperature the product crystallised. The solid product was collected by filtration, washed with DMF.DMA and then ether and dried under vacuum at 40° C. to give the title compound (1.55 g, 47%) as a pale brown crystalline solid. NMR: 1.72 (m, 2H), 2.28 (m, 2H), 2.39 (s, 3H), 2.64 (m, 2H), 2.95 (m, 6H), 5.22 (m, 1H), 5.50 (d, 1H), 7.39 (s, 1H), 7.51 (d, 1H).