反应详情

温度

90 °C

To a solution of 2-(2-chloro-pyrimidin-5-yl)-1-oxo-2,8-diaza-spiro[4.5]decane-8-carboxylic acid tert-butyl ester (102 mg, 0.28 mmol) in DMSO (2 mL) was added (2S,3′S)-2-methyl-[1,3′]bipyrrolidinyl hydrochloride (350 mg, 1.23 mmol), and K2CO3 (920 mg, 6.65 mmol). The reaction mixture was heated to 90° C. with stirring for 18 hours. The reaction was cooled to rt and was added NaHCO3 (aq) (10 mL), extracted with EtOAc (2×10 mL), washed organics with brine (5 mL), concentrated and purified by flash column chromatography (5% 7N NH3 in MeOH/CH2Cl2) to obtain 18.9 mg (15% yield) of the title compound.

1. temperatureThe reaction was cooled to rt
2. extractionextracted with EtOAc (2×10 mL)
3. washwashed organics with brine (5 mL)
4. concentrationconcentrated
5. custompurified by flash column chromatography (5% 7N NH3 in MeOH/CH2Cl2)