反应详情

温度

40 °C

To a solution of 3 (800 mg, 2.73 mmol) in water (15 mL) in a 20 mL microwave reaction vessel was added DIPEA (1.2 mL, 6.8 mmol) and a stir bar. The reaction vessel was sealed and the immiscible slurry was shaken vigorously before insertion in the microwave oven cavity. After 1 min of pre-stirring, the reaction was irradiated for 40 min to a set temperature of 100° C. After cooling to 40° C., the transparent solution was concentrated in vacuo, and the residual brown oil co-evaporated 3 times with MeCN to remove any residual water. The crude product 4, in the form of a DIPEA salt, was immediately taken forward to the next step. LC/MS (Method A): tR=1.29 min, >95%, m/z (ESI+)=312 (MH+).

1. customThe reaction vessel was sealed
2. stirringAfter 1 min of pre-stirring
3. customthe reaction was irradiated for 40 min to a set temperature of 100° C
4. concentrationthe transparent solution was concentrated in vacuo
5. customto remove any residual water