反应详情

To a solution of NaH (146 mg, 6.06 mmol) in DMF (3 mL) was added 1-methyl-1H-indazol-6-ol (300 mg, 2.02 mmol) at 25° C. After stirring for 5 minutes, ethyl 2-bromoacetate (406 mg, 2.43 mmol) was added and stirred for 16 h at 25° C. The mixture was then diluted with water (50 mL) and washed with ethyl acetate (2×20 mL). The water layer was then acidified by adding with 2N HCL until pH3 and then extracted with ethylacetate (2×20 ml). The combined organic layers were washed with brine (30 mL), dried over Na2SO4 and concentrated to give the crude product (300 mg, 63.4%) as colorless oil. It was used in next step without further purification. LCMS (m/z): 207.1 (M+1).

1. stirringstirred for 16 h at 25° C
2. washwashed with ethyl acetate (2×20 mL)
3. additionby adding with 2N HCL until pH3
4. extractionextracted with ethylacetate (2×20 ml)
5. washThe combined organic layers were washed with brine (30 mL)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated