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1-(6-chloropyridin-3-yl)piperazine (250 mg, 1265 μmol) and dimethylaminoacetyl chloride hydrochloride, 85% (260 mg, 1644 μmol) were dissolved in DMF (6 mL) and DIEA (661 μl, 3794 μmol).). The reaction was stirred at room temperature for 4 hours and then 20 hours at 60° C. The resulting solution was taken up in ethyl acetate 80 mL) and washed with aqueous K2CO3 (10%, 70 mL), water (70 mL), and brine (70 mL). The organic phase was dried (MgSO4) and evaporated to give a brown oil. Silica gel chromatography (gradient elution dichloromethane/0-10% 2M NH3 in methanol) afforded compound 300 as an orange tar (174 mg, 49%).

1. custom20 hours
2. customat 60° C
3. washwashed with aqueous K2CO3 (10%, 70 mL), water (70 mL), and brine (70 mL)
4. dry with materialThe organic phase was dried (MgSO4)
5. customevaporated
6. customto give a brown oil
7. washSilica gel chromatography (gradient elution dichloromethane/0-10% 2M NH3 in methanol)