تفاعل #90751

معادلة التفاعل

ethyl 2-oxopiperidine-4-carboxylate

Lawesson's reagent

→

ethyl 2-thioxopiperidine-4-carboxylate

المردود 49.3%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was heated
2. 2
   درجة الحرارةto reflux for 2 h
3. 3
   أخرىRemoved the solvent under reduced pressure
4. 4
   أخرىthe residue was purified by silica gel column chromatography (DCM/EA=20/1)

الإجراء التجريبي

To a solution of ethyl 2-oxopiperidine-4-carboxylate (10.76 g, 62.85 mmol) in toluene (120 mL) was added the Lawesson's reagent (25.42 g, 62.85 mmol) under a nitrogen atmosphere. The mixture was heated to reflux for 2 h. Removed the solvent under reduced pressure and the residue was purified by silica gel column chromatography (DCM/EA=20/1) to afford ethyl 2-thioxopiperidine-4-carboxylate (5.8 g, yield 49.3%).

المصدر