반응 #640584

반응 방정식

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

수율 92.1%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도cooled
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The organic layer was washed with a saturated brine
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타the solvent was evaporated under reduced pressure
6. 6
   기타The obtained crude crystal
7. 7
   세척was washed with a mixture of hexane-ether (2:1)

실험 절차

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).

출처