反应详情

A mixture of 6.81 g of 4-amino-4-phenylpiperidine dibenzenesulfonate, 5.2 g of the compound obtained in step B of EXAMPLE 1 and 6.1 g of K2CO3 in 30 ml of a DMF/acetonitrile mixture (50/50; v/v) is heated at 1 00° C. for 5 hours. It is concentrated under vacuum, the residue is taken up with water and extracted with AcOEt, the organic phase is washed with water 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 DCM/MeOH mixture (from 99/1; v/v to 85/15; v/v) as the eluent to give 3.6 g of the expected product.

1. temperatureis heated at 1 00° C
2. concentrationIt is concentrated under vacuum
3. extractionextracted with AcOEt
4. washthe organic phase is washed with water and with saturated NaCl solution
5. dry with materialdried over MgSO4
6. customthe solvent is evaporated off under vacuum
7. customThe residue is chromatographed on silica H