反应 #2122480

反应方程式

1-Methoxy-4-trimethylsilanyloxy-piperidine-4-carbonitrile

HCl

Sodium hydrogen sulfate

→

4-hydroxy-1-methoxy-piperidine-4-carbonitrile

溶剂

water

反应条件

后处理

1. 1
   萃取The aqueous layer was carefully extracted with ethyl acetate three times
2. 2
   干燥dried over magnesium sulfate
3. 3
   浓缩concentrated
4. 4
   其他The crude product (ca 94% pure) was used directly for the next step without further purification

实验过程

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.

来源