Реакция #2122480
ord-04a7f95571e44b189f82c934de6ce355
Уравнение реакции
1-Methoxy-4-trimethylsilanyloxy-piperidine-4-carbonitrile
HCl
Sodium hydrogen sulfate
→
4-hydroxy-1-methoxy-piperidine-4-carbonitrile
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ЭкстракцияThe aqueous layer was carefully extracted with ethyl acetate three times
- 2Сушкаdried over magnesium sulfate
- 3Концентрированиеconcentrated
- 4ДругоеThe crude product (ca 94% pure) was used directly for the next step without further purification
Методика
1-Methoxy-4-trimethylsilanyloxy-piperidine-4-carbonitrile (1.0 g, 4.4 mmol) was slowly added to aqueous HCl (3N) at 15° C. The mixture was stirred for two hours at room temperature and then poured into cold (0° C.) water. Sodium hydrogen sulfate (saturated aqueous solution) was slowly added to adjust the pH to 7. The aqueous layer was carefully extracted with ethyl acetate three times. All organic layers were combined, dried over magnesium sulfate and concentrated. The crude product (ca 94% pure) was used directly for the next step without further purification. Yield: 500 mg of 4-hydroxy-1-methoxy-piperidine-4-carbonitrile (compound P4.2) as light yellow solid.