反应详情

To a solution of (R)-piperidine-3-carboxylic acid (2.0 g, 15.48 mmol) in water (40 mL) and THF (20 mL) were added NaHCO3 (3.30 g, 38.70 mmol) and 3-methylbutanoyl chloride (2.8 mL, 23.2 mmol) at room temperature. The reaction was stirred overnight, concentrated under reduced pressure, diluted with water (50 mL) and extracted with EtOAc (1×). The aqueous layer was acidified with 1N HCl, extracted with EtOAc (3×) and the combined extracts were dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound (2.53 g, 76%). MS 214 (MH+).

1. concentrationconcentrated under reduced pressure
2. additiondiluted with water (50 mL)
3. extractionextracted with EtOAc (1×)
4. extractionextracted with EtOAc (3×)
5. dry with materialthe combined extracts were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure