反应详情

温度

55 °C

To a solution of 7-(2-fluoro-4-methylsulfanyl-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid methyl ester (635 mg, 1.9 mmol) in dioxane (8 mL) and water (2.5 mL) was added lithium hydroxide monohydrate (161 mg, 3.8 mmol). The reaction was stirred at 55° C. for 2 hours then cooled to room temperature. Aqueous hydrochloric acid (1M) was added dropwise until pH˜3. The reaction mixture was extracted twice with ethyl acetate (2×10 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo to give the title compound as a dark brown solid (600 mg, 99%). LCMS (Method B): RT=3.20 min, M+H+=318.

1. temperaturethen cooled to room temperature
2. extractionThe reaction mixture was extracted twice with ethyl acetate (2×10 mL)
3. washThe combined organic fractions were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo