反应 #640581

反应方程式

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

收率 63.2%

溶剂

ethanol

反应条件

后处理

1. 1
   温度to reflux for one hour
2. 2
   过滤the reaction mixture was filtered with suction
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤The organic layer was washed with a saturated brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他the solvent was evaporated under reduced pressure

实验过程

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).

来源