تفاعل #323291

معادلة التفاعل

3-[(4-chlorophenyl)sulfonyl]pyrrolidine

tetrahydrofuran

1,1'-carbonyldiimidazole

N,N-diethylaminoethylamine

tetrahydrofuran

→

white crystals

المردود 46.7%

3-[(4-Chlorophenyl)sulfonyl]-N-[2-(diethylamino)ethyl]-1-pyrrolidinecarboxamide

المردود 46.7%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe solution was refluxed overnight
2. 2
   أخرىThe solvent was removed in vacuo
3. 3
   workup.DISSOLUTIONthe resulting oil was dissolved in methylene chloride
4. 4
   استخلاصThe solution was extracted with several portions of water
5. 5
   تجفيفwas dried over magnesium sulfate
6. 6
   أخرىThe solvent was removed in vacuo
7. 7
   أخرىto give an oil residue
8. 8
   أخرىThe residue was crystallized from a mixture of methanol, ether and hexane

الإجراء التجريبي

A solution of 4.93 g (0.0304 mole) of 1,1'-carbonyldiimidazole and 3.36 g (0.029 mole) of N,N-diethylaminoethylamine in 200 ml of tetrahydrofuran was stirred for 40 min at room temperature. A solution of 5.78 g (0.0236 mole) of 3-[(4-chlorophenyl)sulfonyl]pyrrolidine (free base) in tetrahydrofuran was added and the solution was refluxed overnight. The solvent was removed in vacuo and the resulting oil was dissolved in methylene chloride. The solution was extracted with several portions of water and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil residue. The residue was crystallized from a mixture of methanol, ether and hexane to give 4.28 g (46.7%) of white crystals, m.p. 86°-87.5° C.

المصدر