反应详情

温度

0 °C

A mixture of 4-{1,3-dimethyl-1H-pyrazolo[4,3-d]pyrimidin-7-yl}-6-[2-(1-methylisoquinolin-6-yl)ethynyl]pyridin-2-amine (30 mg, 74 μmol), toluene (200 μl) and DIPEA (57 μl, 333 μmol) is cooled to 0° C. 2-Bromobutanoyl bromide (29 μl, 0.24 mmol) in toluene (200 μl) is added dropwise. The mixture is warmed to 50° C. and stirring is continued for 16 h. Cooled to RT 2-bromobutanoyl bromide (29 μl, 0.24 mmol) in toluene (200 μl) is added dropwise. The mixture is stirred at 60° C. for 16 h before it is again cooled to RT. Ethanamine (aqueous solution 70 wt.-%, 1 ml) is added and the mixture stirred for 16 h at 80° C. The mixture is concentrated in vacuo and the product purified by RP HPLC. Yield: 3 mg (8%). HPLC-MS: M+H=519; tR=1.37 min (METHOD—1).

1. temperatureThe mixture is warmed to 50° C.
2. additionis added dropwise
3. stirringThe mixture is stirred at 60° C. for 16 h before it
4. temperatureis again cooled to RT
5. stirringthe mixture stirred for 16 h at 80° C
6. concentrationThe mixture is concentrated in vacuo
7. customthe product purified by RP HPLC