反应详情

N-[2-(5-Amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide (80 mg, 0.25 mmol) and lithium aluminum hydride (92 mg) were refluxed in anhydrous THF (10 mL) for 3 hrs. The resulting mixture was poured into a saturated ammonium chloride solution (50 mL). The aqueous phase was extracted with ethyl acetate (3×50 mL). The combined extracts were washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated to yield 54 mg of crude product. The crude product was purified by flash column chromatography eluting with CH2Cl2:MeOH=5:1 with 0.5% NH3. The title compound was isolated in a yield of 36 mg (48%). MS (m/z, ES+): 303.1 (M+1, 100%).

1. extractionThe aqueous phase was extracted with ethyl acetate (3×50 mL)
2. washThe combined extracts were washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customevaporated
6. customto yield 54 mg of crude product
7. customThe crude product was purified by flash column chromatography
8. washeluting with CH2Cl2