반응 #640581

반응 방정식

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

수율 63.2%

용매

ethanol

반응 조건

후처리

1. 1
   온도to reflux for one hour
2. 2
   여과the reaction mixture was filtered with suction
3. 3
   추출extracted with ethyl acetate
4. 4
   세척The organic layer was washed with a saturated brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   기타the solvent was evaporated under reduced pressure

실험 절차

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).

출처