反应详情

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+).

1. additionAfter completion of addition the reaction mixture
2. temperaturewas heated to reflux
3. customquenched with water
4. extractionThe aqueous layer was extracted with ethyl acetate (3×100 mL)
5. dry with materialThe combined organic layers were dried over sodium sulfate
6. concentrationconcentrated
7. customto yield an oil
8. customThis crude material was purified