反应 #640584

反应方程式

4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride

2-Nitrobenzyl amine hydrochloride

3-hydroxy-3-phenyl propionic acid

triethylamine

hydrochloric acid water

→

3-hydroxy-N-(2-nitrobenzyl)-3-phenyl propionic acid amide

收率 92.1%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度cooled
2. 2
   萃取extracted with ethyl acetate
3. 3
   洗涤The organic layer was washed with a saturated brine
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他the solvent was evaporated under reduced pressure
6. 6
   其他The obtained crude crystal
7. 7
   洗涤was washed with a mixture of hexane-ether (2:1)

实验过程

2-Nitrobenzyl amine hydrochloride (2.27 g, 12.0 mmol), 3-hydroxy-3-phenyl propionic acid (2.00 g, 12.0 mmol), triethylamine (1.34 g, 13.3 mmol) were added to tetrahydrofuran (50 ml) and the reaction mixture was ice cooled. Under ice cooled condition, 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (3.33 g, 12.0 mmol) was added thereto and stirred at room temperature for five hours. The reaction mixture was poured into dilute hydrochloric acid water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained crude crystal was washed with a mixture of hexane-ether (2:1) to obtain 3-hydroxy-N-(2-nitrobenzyl)-3-phenyl propionic acid amide (3.32 g).

来源