反应详情

温度

60 °C

A mixture of 0.53 g of 4-phenyl-1-azabicyclo[2.2.2]octane and 1.4 g of the compound obtained in step C of EXAMPLE 4 in 5 ml of DMF is heated at 60° C. for 5 hours. After cooling to RT, the reaction mixture is poured into water and extracted with DCM, the organic phase is washed twice with 2N HCl solution and three times with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using DCM and then a DCM/MeOH mixture (92/8; v/v) as the eluent. The product obtained is taken up with ether and the precipitate formed is wrung to give 0.21 g of the expected product. M.p.=138° C.

1. temperatureAfter cooling to RT
2. extractionextracted with DCM
3. washthe organic phase is washed twice with 2N HCl solution and three times with saturated NaCl solution
4. dry with materialdried over MgSO4
5. customthe solvent is evaporated off under vacuum
6. customThe residue is chromatographed on silica
7. customThe product obtained
8. customthe precipitate formed