反应详情

温度

0 °C

To a solution of Boc-L-Proline (4.5 g, 0.02 mmol) and pyridine (8.45 mL, 0.104 mmol) in DCM (20 mL) cooled in an ice bath was added dropwise cyanuric fluoride (5.35 mL, 0.0627 mmol). After the addition the reaction became milky. The solution was stirred at 0° C. for 10 min then warmed to RT and stirred for 4 h. The reaction was quenched with water, and thrice extracted with DCM. The combined organic extracts were washed with brine, dried, and concentrated in vacuo to afford tert-butyl 2-(fluorocarbonyl)pyrrolidine-1-carboxylate. The crude acid fluoride was used in next coupling reaction immediately.

1. additionAfter the addition the reaction
2. temperaturethen warmed to RT
3. stirringstirred for 4 h
4. customThe reaction was quenched with water, and thrice
5. extractionextracted with DCM
6. washThe combined organic extracts were washed with brine
7. customdried
8. concentrationconcentrated in vacuo