反应详情

To a solution of 4-bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1-sulfonic acid dimethylamide (3.85 g, 11.2 mmol) in MeOH (50 ml) at 0° C. was added 6 N HCl (50 mL). The reaction was warmed to room temperature and stirred overnight. The reaction was quenched by adding concentrated NH4OH until a pH of 8 was obtained. After concentrating to remove the MeOH, the remaining reaction solution was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The crude product was purified over normal phase silica starting with 10% EtOAc in heptane for 5 m and then increasing to 100% EtOAc over 40 m to give the desired product as a clear oil (2.42 g, 10.2 mmol). MS m/z 239.3 (M+H)+.

1. customThe reaction was quenched
2. additionby adding concentrated NH4OH until a pH of 8
3. customwas obtained
4. concentrationAfter concentrating
5. customto remove the MeOH
6. customthe remaining reaction solution
7. extractionwas extracted with EtOAc
8. dry with materialthe organic layer was dried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated
11. customThe crude product was purified over normal phase silica starting with 10% EtOAc in heptane for 5 m
12. temperatureincreasing to 100% EtOAc over 40 m