反应详情

温度

90 °C

A mixture of 0.44 g of 4-(acetylamino)-4-benzylpiperidine p-toluene-sulfonate, 0.50 g of the compound obtained in step B of EXAMPLE 1 and 0.53 g of K2CO3 in 5 ml of DMF is heated at 90° C. for 2 hours. The reaction mixture is poured into water and extracted with AcOEt, the organic phase is washed with 2 N NaOH and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using a gradient of a DCM/MeOH mixture (99/1; v/v to 93/7; v/v) as the eluent. The product obtained is dissolved in DCM and acidified by the addition of ethereal hydrogen chloride and the precipitate formed is filtered off to give 0.38 g of the expected product, m.p=158° C. (dec.).

1. extractionextracted with AcOEt
2. washthe organic phase is washed with 2 N NaOH and with saturated NaCl solution
3. dry with materialdried over MgSO4
4. customthe solvent is evaporated off under vacuum
5. customThe residue is chromatographed on silica H
6. customThe product obtained
7. customthe precipitate formed
8. filtrationis filtered off