反应详情

A mixture of 4-Methyl-2-{2-[1-(tetrahydro-pyran-2-yl)-1H-indazol-4-yl]-acetylamino}-thiazole-5-carboxylic acid ethyl ester (800 mg, 1.867 mmol), lithium hydroxide monohydrate (394 mg, 9.391 mmol), ethanol (8 mL) and water (24 mL) was placed in an oil bath preheated to 90° C. and the resulting solution was heated for 28 min. The reaction solution was diluted with water (20 mL), saturated with sodium chloride, acidified with aqueous 2N HCl and extracted with 4/1 ethyl acetate/THF (4×100 mL). The organic layers were combined, washed with brine (50 mL), dried over MgSO4, filtered and concentrated under reduced pressure to give 4-Methyl-2-{2-[1-(tetrahydro-pyran-2-yl)-1H-indazol-4-yl]-acetylamino}-thiazole-5-carboxylic acid (0.54 g, 72.2%) as a yellow solid. MS m/e 401.4 (M+H+).

1. customwas placed in an oil bath
2. custompreheated to 90° C.
3. temperaturethe resulting solution was heated for 28 min
4. extractionextracted with 4/1 ethyl acetate/THF (4×100 mL)
5. washwashed with brine (50 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure