反应 #1810841

ord-0ffa5dac74b64c51b39a39b1efa6292b

反应方程式

CC(=O)c1cn(C2CCC2)c(C)n1
1-Cyclobutyl-2-methyl-4-acetylimidazole
CN(C)C=O
DMF
CC(=O)N(C)C
DMA
Cc1ncc(C(=O)C=CN(C)C)n1C1CCC1
title compound
收率 47.0%
Cc1ncc(C(=O)C=CN(C)C)n1C1CCC1
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. 1
    温度at reflux, under an atmosphere of nitrogen, for 54 hours
  2. 2
    其他crystallised
  3. 3
    过滤The solid product was collected by filtration
  4. 4
    洗涤washed with DMF
  5. 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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07485638B2uspto-grants-2009_02