反応 #2122480

反応方程式

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

HCl

Sodium hydrogen sulfate

→

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

溶媒

water

反応条件

後処理

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

実験手順

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.

出典