反应详情

温度

80 °C

A mixture of 0.98 g of the compound obtained in step B of EXAMPLE 14, 0.645 g of 4-phenyl-4-(pyrrolidin-1-ylcarbonyl)piperidine and 0.69 g of K2CO3 in 3 ml of DMF is heated at 80° C. for 2 hours. After cooling to RT, the reaction mixture is poured into water and extracted with an AcOEt/ether mixture, the organic phase is washed with water and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using a DCM/MeOH mixture (100/2; v/v) as the eluent. The product obtained is dissolved in the minimum amount of DCM and acidified to pH 1 by the addition of a saturated solution of gaseous HCl in ether and the precipitate formed is wrung to give 0.42 g of the expected product. M.p.=155°-178° C.

1. temperatureAfter cooling to RT
2. extractionextracted with an AcOEt/ether mixture
3. washthe organic phase is washed with water
4. dry with materialdried over MgSO4
5. customthe solvent is evaporated off under vacuum
6. customThe residue is chromatographed on silica H
7. customThe product obtained
8. customthe precipitate formed