تفاعل #1681981

معادلة التفاعل

3-(4-bromobutyl)-1-thia-3-azaspiro[4.5]decan-4-one

1-(4-fluorophenyl)-3-piperazino-1H-indole

K2CO3

NaI

→

crystals

المردود 43.6%

3-[4-[1-[1-(4-Fluorophenyl)-1H-indol-3-yl]-4-piperazinyl]butyl]-1-thia-3-azaspiro[4.5]decan-4-one

المردود 43.6%

المذيبات

CH3CN

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled to room temperature
2. 2
   ترشيحfiltered
3. 3
   تركيزthe filtrate concentrated in vacuo
4. 4
   أخرىThe residue was chromatographed on silica
5. 5
   workup.ADDITIONThe fractions containing the desired product
6. 6
   تركيزconcentrated
7. 7
   أخرىto provide a foam which
8. 8
   أخرىwas recrystallized from ether

الإجراء التجريبي

A mixture of 3-(4-bromobutyl)-1-thia-3-azaspiro[4.5]decan-4-one (3.8 g), 1-(4-fluorophenyl)-3-piperazino-1H-indole (3.7 g), K2CO3 (3.5 g), NaI (200 mg) and anhydrous CH3CN (150 ml) was heated to 80° C. with stirring under nitrogen. After 18 hours, no starting amine remained as judged by TLC. The mixture was cooled to room temperature and filtered, and the filtrate concentrated in vacuo. The residue was chromatographed on silica using EtOAc as an eluent. The fractions containing the desired product were combined and concentrated to provide a foam which was recrystallized from ether to provide 2.816 g of crystals, m.p. 134-136° C., homogeneous by TLC.

المصدر