反应详情

温度

4 °C

5-(3,5-Difluoro-benzyloxy)-1H-indazol-3-ylamine (550 mg, 2 mmol) was dissolved in sym-collidine, cooled to 4° C. and treated with neat 3-chloromethyl-benzoyl chloride (0.34 mL, 2.4 mmol). After 1 hour the reaction mixture was added drop wise into iced water, with stirring and separation of a yellow oil occurred. Then, EtOAc (50 mL) and 2N HCl (25 mL) were added. The organic phase was separated, washed with aqueous NaHCO3 (50 mL), brine, dried over sodium sulfate and evaporated to dryness. After purification over silica gel (eluent: DCM:MeOH 95:5) 378 mg of title compound were obtained as a whitish solid in 56% yield.

1. customseparation of a yellow oil
2. additionThen, EtOAc (50 mL) and 2N HCl (25 mL) were added
3. customThe organic phase was separated
4. washwashed with aqueous NaHCO3 (50 mL), brine
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness
7. customAfter purification over silica gel (eluent: DCM:MeOH 95:5) 378 mg of title compound
8. customwere obtained as a whitish solid in 56% yield