반응 #78933

반응 방정식

1-(2-methoxy-phenyl) piperazine

3-methanesulfonyloxymethyl-piperidine-1-carboxylic acid tert-butyl ester

potassium carbonate

→

desired compound

3-[4-(2-Methoxy-phenyl)-piperazin-1-ylmethyl]-piperidine-1-carboxylic acid tert-butyl ester

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONAfter completion of addition the reaction mixture
2. 2
   온도was heated to reflux
3. 3
   기타quenched with water
4. 4
   추출The aqueous layer was extracted with ethyl acetate (3×100 mL)
5. 5
   건조The combined organic layers were dried over sodium sulfate
6. 6
   농축concentrated
7. 7
   기타to yield an oil
8. 8
   기타This crude material was purified

실험 절차

To a solution of 3-methanesulfonyloxymethyl-piperidine-1-carboxylic acid tert-butyl ester (11.06 g, 0.04 mol) in acetonitrile (180 mL) was added potassium carbonate (26 g, 0.19 mol) followed by 1-(2-methoxy-phenyl) piperazine (7.25 g, 0.04 mol). After completion of addition the reaction mixture was heated to reflux. After 12 h the reaction mixture was cooled down to room temperature and quenched with water. The aqueous layer was extracted with ethyl acetate (3×100 mL). The combined organic layers were dried over sodium sulfate and concentrated to yield an oil. This crude material was purified using silica gel chromatography (7:3:0.05 Hexane:EtOAc:2M NH3 in EtOH) to afford the desired compound in good yield (8.0 g, 55%). C22H35N3O3,LRMS (m/z)=390 (MH+).

출처