反应详情

Add 22 mg (0.54 mmol) sodium hydride (60% dispersion in mineral oil) to a solution of 100 mg (0.43 mmol) 4-{[(2S)-2-hydroxypropyl](methyl)amino}butyric acid tert.-butyl ester in 1 ml THF, with ice cooling. After stirring for ten minutes with ice cooling, add a solution of 161 mg (0.45 mmol) 4-chloro-6-(2-fluorophenyl)-5-(4-methoxyphenyl)furo[2,3-d]pyrimidine in 2 ml THF and 8 mg (0.02 mmol) tetra-n-butylammonium iodide. Stir the reaction mixture for 16 hours at room temperature. After adding water and ethyl acetate, wash the separated organic phase with 1 N hydrochloric acid and concentrate by vacuum evaporation. Take up the residue in acetonitrile/DMSO and purify by preparative RP-HPLC (gradient: water/acetonitrile). 114 mg (93% purity, 45% of theor.) of the desired product is obtained.

1. stirringStir the reaction mixture for 16 hours at room temperature
2. washwash the separated organic phase with 1 N hydrochloric acid
3. concentrationconcentrate by vacuum evaporation
4. custompurify by preparative RP-HPLC (gradient: water/acetonitrile)