HRID2246613
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 1,1-dimethylethyl 5-{5-[(cyclopropylamino)carbonyl]-3-fluoro-2-methylphenyl}-1H-indazole-1-carboxylate (Intermediate 2, 0.46 g) in a solution of hydrogen chloride in dioxan (4M, 7 ml) was stirred at room temperature. under nitrogen for 4.5 h. The solvent was evaporated and the residue was partitioned between dichloromethane (20 ml) and aqueous sodium hydroxide (2M, 20 ml). The organic layer was separated using a hydrophobic filter tube, the solvent was evaporated and the residue was purified on a Varian Bond-Elut SPE cartridge (silica, 10 g) eluting with chloroform:methanol (100:0 to 98:2) to give the title compound (0.06 g).
WORKUP
后处理
- customThe solvent was evaporated
- customthe residue was partitioned between dichloromethane (20 ml) and aqueous sodium hydroxide (2M, 20 ml)
- customThe organic layer was separated
- customthe solvent was evaporated
- customthe residue was purified on a Varian Bond-Elut SPE cartridge (silica, 10 g)
- washeluting with chloroform:methanol (100:0 to 98:2)