反应 #1340631

反应方程式

methyl[(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate

1-pyridin-2-ylmethanamine

→

methyl[(4Z)-1-methyl-5-oxo-4-{1-[(pyridin-2-ylmethyl)amino]pentylidene}-4,5-dihydro-1H-pyrazol-3-yl]acetate

收率 92.0%

溶剂

toluene

反应条件

后处理

1. 1
   workup.ADDITIONThe mixture of the
2. 2
   其他The solvent was removed in vacuo
3. 3
   workup.DISSOLUTIONThe resulting residue was dissolved in a minimum of CH2Cl2
4. 4
   workup.ADDITIONadded dropwise to a stirred solution of 200 mL of cyclohexane resulting in the formation of a brown precipitate that
5. 5
   过滤was filtered off

实验过程

The mixture of the above obtained methyl[(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate (Compound of Formula (VII), 1.05 g) and 1-pyridin-2-ylmethanamine (0.262 mL) was stirred at room temperature in toluene (25 mL) for 0.5 h. The solvent was removed in vacuo. The resulting residue was dissolved in a minimum of CH2Cl2 and added dropwise to a stirred solution of 200 mL of cyclohexane resulting in the formation of a brown precipitate that was filtered off. This precipitate was proved to be the pure methyl[(4Z)-1-methyl-5-oxo-4-{1-[(pyridin-2-ylmethyl)amino]pentylidene}-4,5-dihydro-1H-pyrazol-3-yl]acetate (1.20 g). Yield 92%. MS (ESI+): 345.4; MS (ESI−): 342.5.

来源