反应详情

温度

-35 °C

To a stirred solution of (5R)-1-(chloroacetyl)-5-ethynyl-L-prolinamide (0.16 g, 0.745 mmol) and imidazole (0.05 g, 0.745 mmol) in dry pyridine (4 mL) at −35° C. under nitrogen was added POCl3 (0.15 mL, 1.49 mmol) dropwise. The reaction mixture was stirred between −35° C. to ±15° C. for 1 hour and evaporated. The residue was diluted with dichloromethane and washed with H2O (2×), dried (Na2SO4), filtered and concentrated under reduced pressure. Purification by flash chromatography (10% ethyl acetate/hexane) provided the titled compound. MS (CI) m/z 197 (M+1)+.

1. customevaporated
2. additionThe residue was diluted with dichloromethane
3. washwashed with H2O (2×)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customPurification by flash chromatography (10% ethyl acetate/hexane)