反应详情

A suspension of sodium dithionite (524 mg, 3.48 mmol) and 4-(2-fluoro-4-iodo-phenylamino)-6-methoxy-5-nitro-indazole-1-carboxylic acid tert-butyl ester (434 mg, 0.87 mmol) in water (10 mL) was treated with a 1:1 mixture of THF:dioxane (10 mL). The homogeneous reaction mixture stirred at room temperature for 18 hours. The reaction mixture was basified by the addition of saturated aqueous sodium hydrogen carbonate and then extracted twice with ethyl acetate. The combined organic extracts were washed with water, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a yellow solid (300 mg, 73%). LCMS (Method B) RT 4.16 min, [M+H]+=499 [M−H]−=497.

1. extractionextracted twice with ethyl acetate
2. washThe combined organic extracts were washed with water
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo