反应详情

A mixture of 1.1 g of the compound obtained in step B of EXAMPLE 14, 1.2 g of 4-phenyl-4-(pyrrolidin-1-ylcarbonylamino)piperidine benzenesulfonate and 0.95 g of K2CO3 in 3 ml of DMF is heated at 80°-100° C. for 3 hours. After cooling to RT, the reaction mixture is poured into water and the precipitate formed wrung, washed with water and dried under vacuum The precipitate is chromatographed on silica H using a DCM/MeOH mixture (from 100/2; v/v to 100/3; 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 0.54 g of the expected product. M.p.=158°-160° C.

1. temperatureis heated at 80°-100° C. for 3 hours
2. customthe precipitate formed wrung
3. washwashed with water
4. customdried under vacuum The precipitate
5. customis chromatographed on silica H
6. customThe product obtained
7. customthe precipitate formed