反应详情

温度

65 °C

A mixture of 1.6 g (4 mmol) [6-(4-chloromethyl-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-((R)-1-phenyl-ethyl)-amine (for the preparation see Example 9, Step 9.3 of WO 03/013541 A1) in 50 ml DMF is treated with 1.56 g (8.4 mmol) N—BOC-piperazine and 2.76 g (20 mmol) anhydrous potassium carbonate and the mixture heated to 65° C. for 1 hour. The reaction mixture is cooled and the inorganic salts removed by filtration (Hyflo Super Cel®; Fluka, Buchs, Switzerland). The DMF is evaporated under reduced pressure and the residue purified through flash chromatography using first dichloromethane/ethanol 95:5 and then dichloromethane/ethanol 9:1. The title compound is obtained as a solid; m.p. 244-246° C.; MS-ES+: (M+H)+=513; TLC Rf(dichloromethane/ethanol 9:1) 0.46.

1. temperatureThe reaction mixture is cooled
2. customthe inorganic salts removed by filtration (Hyflo Super Cel®; Fluka, Buchs, Switzerland)
3. customThe DMF is evaporated under reduced pressure
4. customthe residue purified through flash chromatography