Reaktion #640581

Reaktionsgleichung

5,5-Dimethyl-3-(2-nitrobenzyl)-[1,3]-oxazinan-2-thione

ammonium chloride

water

→

3-(2-aminobenzyl)-5,5-dimethyl-[1,3]-oxazinan-2-thione

Ausbeute 63.2%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for one hour
2. 2
   Filtrationthe reaction mixture was filtered with suction
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with a saturated brine
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

5,5-Dimethyl-3-(2-nitrobenzyl)-[1,3]-oxazinan-2-thione (1.06 g, 3.79 mmol), iron powder (1.06 g, 19.0 mmol), ammonium chloride (0.10 g, 1.87 mmol) were suspended in ethanol (20 ml) and water (10 ml) and heated to reflux for one hour. After cooling to room temperature, the reaction mixture was filtered with suction 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 to obtain 3-(2-aminobenzyl)-5,5-dimethyl-[1,3]-oxazinan-2-thione (0.60 g).

Quelle