反应详情

温度

0 °C

1.8 g (11.6 mmol) (pyridin-3-yloxy)-acetic acid and 1.7 ml (12.2 mmol) TEA are suspended in 80 ml absolute dichlormethane and cooled to ca. 0° C. under moisture exclusion. 2.1 g (13.7 mmol) 88% HOBT and 2.7 g (14.1 mmol) EDC are added and the mixture is stirred for 30 min under ice-cooling. 4,. g (13.0 mmol) 4-[4-(hydroxy-diphenylmehyl)-piperidin-1-yl]-butylamine are added and the mixture is stirred overnight without cooling. Subsequently, the batch is washed with 50 ml 1M sodium hydroxide solution and twice each with 30 ml water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum. The residue is chromatographically purified over silica gel with CHCl3/CH3OH/NH4OH (90/10/0 to 90/10/1): Yield 2.0 g (34%) of a colorless resin.

1. temperaturecooling
2. stirringthe mixture is stirred overnight
3. temperaturewithout cooling
4. washSubsequently, the batch is washed with 50 ml 1M sodium hydroxide solution
5. dry with materialThe organic phase is dried over sodium sulfate
6. customthe solvent is removed under vacuum
7. customThe residue is chromatographically purified over silica gel with CHCl3/CH3OH/NH4OH (90/10/0 to 90/10/1)