Реакция #640581
ord-3d9c03ae6eaf484aa6d10801236b1507
Уравнение реакции
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
Выход 63.2%
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураto reflux for one hour
- 2Фильтрацияthe reaction mixture was filtered with suction
- 3Экстракцияextracted with ethyl acetate
- 4ПромывкаThe organic layer was washed with a saturated brine
- 5Сушкаdried over anhydrous sodium sulfate
- 6Другоеthe solvent was evaporated under reduced pressure
Методика
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).