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
DMF (1 ml) was added to 3-methyl-2-(methyloxy)benzoic acid (134 mg, 0.81 mmol) (Apin Chemicals), HATU (306 mg, 0.81 mmol) and DIPEA (0.422 ml, 2.417 mmol). The reaction was stirred for 30 mins under nitrogen before addition of 6-(1H-indol-4-yl)-1H-indazol-4-amine (100 mg, 0.403 mmol). The reaction was stirred under nitrogen at RT overnight, then it was loaded onto a PS-aminopropyl cartridge and left for 3 h. The cartridge was washed with 10% MeOH in DCM. Appropriate fractions were combined and the solvent was evaporated. The residue was dissolved in MeOH:DMSO (2 ml; 1:1, v/v) and purified by Mass Directed Automated Preparative HPLC using method B. The solvent was dried under a stream of nitrogen to give title compound (6 mg).
WORKUP
后处理
- waitleft for 3 h
- washThe cartridge was washed with 10% MeOH in DCM
- customthe solvent was evaporated
- dissolutionThe residue was dissolved in MeOH
- custom1:1, v/v) and purified by Mass Directed Automated Preparative HPLC
- customThe solvent was dried under a stream of nitrogen