Reaktion #640584

Reaktionsgleichung

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

Ausbeute 92.1%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   WaschenThe organic layer was washed with a saturated brine
4. 4
   Trocknendried over anhydrous sodium sulfate
5. 5
   Sonstigethe solvent was evaporated under reduced pressure
6. 6
   SonstigeThe obtained crude crystal
7. 7
   Waschenwas washed with a mixture of hexane-ether (2:1)

Vorschrift

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).

Quelle