反应详情

温度

25 °C

To a 0° C. solution of amide (22) in TFA (1 mL per mmol amide), was added chlorosulfonic acid (2 eq) dropwise under nitrogen atmosphere. The temperature was allowed to warm to 25° C. and stirred for 72 hours. The reaction mixture was quenched by pouring into ice water. The desired product was collected via precipitation from either water/methanol, or ethyl acetate/methanol solution, resulting in a white solid (yield 68%). LC/MS (M+H)+ m/z 346, (M−H)− m/z 344. The crude material was used without further purification.

1. customThe reaction mixture was quenched
2. additionby pouring into ice water
3. customThe desired product was collected via precipitation from either water/methanol, or ethyl acetate/methanol solution