反应详情

温度

70 °C

To 1-tert-butyloxycarbonyl-4-[(4-aminophenyloxy)methyl]piperidine (0.75 g) obtained in Example 13 were added dimethylformamide (10 ml), potassium carbonate (1.4 g) and dibromobutane (0.54 g) and the mixture was heated to 70° C. and stirred overnight. To the reaction solution was added water which was extracted with ethyl acetate (50 ml×3). The combined extract was dried over sodium sulfate and concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate=5/1 (v/v)) to obtain 1-tert-butyloxycarbonyl-4-[(4-pyrrolidinophenyloxy)methyl]piperidine (0.55 g) as colorless crystals, m.p. 141°-145° C.

1. extractionwas extracted with ethyl acetate (50 ml×3)
2. extractionThe combined extract
3. dry with materialwas dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue thus obtained
6. customwas purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate=5/1 (v/v))