반응 #2122480

반응 방정식

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

HCl

Sodium hydrogen sulfate

→

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

용매

water

반응 조건

후처리

1. 1
   추출The aqueous layer was carefully extracted with ethyl acetate three times
2. 2
   건조dried over magnesium sulfate
3. 3
   농축concentrated
4. 4
   기타The crude product (ca 94% pure) was used directly for the next step without further purification

실험 절차

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.

출처