反应详情

温度

150 °C

To 2.70 g (7.81 mmol) {4-[1-(2-chloro-pyrimidin-4-yl)-piperidin-4-yl]-phenyl}-acetic acid methyl ester (XII.2) in 20 mL ACN are added 2.64 mL (23.4 mmol) N-methyl-cyclopentylamine. The mixture is stirred for 2 h at 150° C. under microwave irradiation. After that time, the solvent is evaporated, the residue taken up in 60 mL ethanol and 30 mL 1N NaOH are added. The mixture is stirred for 1 h at rt and for 1 h at 40° C. Subsequently, 30 mL 1N HCl are added, the mixture is concentrated in vacuo and extracted with DCM. The organic layer is dried over sodium sulphate and the solvent is evaporated. The residue is purified by column chromatography (silica gel; DCM:EtOH 80:20) to yield the desired product.

1. customAfter that time, the solvent is evaporated
2. addition30 mL 1N NaOH are added
3. stirringThe mixture is stirred for 1 h at rt and for 1 h at 40° C
4. additionSubsequently, 30 mL 1N HCl are added
5. concentrationthe mixture is concentrated in vacuo
6. extractionextracted with DCM
7. dry with materialThe organic layer is dried over sodium sulphate
8. customthe solvent is evaporated
9. customThe residue is purified by column chromatography (silica gel; DCM:EtOH 80:20)