反应详情

温度

70 °C

To a solution of (2S,3′S)-2-methyl-[1,3′]bipyrrolidinyl (0.072 g, 0.315 mmol) in acetonitrile (25 mL) was added 2-(2-chloro-pyrimidin-5-yl)-8-oxa-2-aza-spiro[4.5]decan-1-one (0.07 g, 0.262 mmol), and powdered potassium carbonate (0.145 g, 1.05 mmol) and stirred at 70° C. for 16.0 hours. Additional (2S,3′S)-2-Methyl-[1,3′]bipyrrolidinyl (0.1 g) was added and reaction mixture stirred for 4 hours at 70° C. The reaction mixture was then allowed to cool to room temperature, quenched with water (2 mL) diluted with ethyl acetate (10 mL). The aqueous phase was extracted with 10% methanol in dichloromethane (10 ml, 3×), combined organics washed with brine, dried over Na2SO4, concentrated under vacuum. Purification by column chromatography on silica gel (0-100%) eluting with methanol in dichloromethane (0-10%) afforded 0.0732 g (72%) of the title compound.

1. customreaction mixture
2. stirringstirred for 4 hours at 70° C
3. temperatureto cool to room temperature
4. customquenched with water (2 mL)
5. additiondiluted with ethyl acetate (10 mL)
6. extractionThe aqueous phase was extracted with 10% methanol in dichloromethane (10 ml, 3×)
7. washcombined organics washed with brine
8. dry with materialdried over Na2SO4
9. concentrationconcentrated under vacuum
10. customPurification by column chromatography on silica gel (0-100%)
11. washeluting with methanol in dichloromethane (0-10%)