反应详情

温度

45 °C

185 mg (0.50 mmol) of (RS)-5-bromo-N4-isopropyl-N2-[4-(methyl sulfinyl)phenyl]-pyrimidine-2,4-diamine in 1 ml of DCM is mixed with 40 mg (0.55 mmol) of sodium azide. The batch is slowly mixed with 0.13 ml of concentrated sulfuric acid at 0° C. and then heated to 45° C. After 16 hours, the batch is cooled to room temperature, mixed with 2 ml of 1N NaOH solution and extracted from ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated by evaporation. The remaining residue is purified by chromatography (DCM/EtOH 9:1). 38 mg (0.10 mmol, corresponding to 20% of theory) of the product is obtained.

1. temperaturethe batch is cooled to room temperature
2. extractionextracted from ethyl acetate
3. dry with materialThe combined organic phases are dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated by evaporation
6. customThe remaining residue is purified by chromatography (DCM/EtOH 9:1)
7. custom38 mg (0.10 mmol, corresponding to 20% of theory) of the product is obtained