反应详情

4.4 250 mg of tert-butyl 3-tert-butoxycarbonylamino-6-ethoxy-7-fluoro-5-[3-(3-fluorobenzyl)ureido]indazole-1-carboxylate (4.5 mmol) are stirred for 16 hours with 5 ml of HCl/dioxane (4 M). The batch is concentrated and evaporated three times with 20 ml of toluene each time in a rotary evaporator. The residue is purified by column chromatography on silica gel (eluent:ethyl acetate:methanol 9:1). Evaporation of the corresponding fractions gives 50 mg of 1-(3-amino-6-ethoxy-7-fluoro-1H-indazol-5-yl)-3-(3-fluorobenzyl)urea (“A14”) (31%), MS-FAB (M+H+)=362.

1. concentrationThe batch is concentrated
2. customevaporated three times with 20 ml of toluene each time
3. customin a rotary evaporator
4. customThe residue is purified by column chromatography on silica gel (eluent:ethyl acetate:methanol 9:1)
5. customEvaporation of the corresponding fractions