反应详情

Lithium hydroxide monohydrate (4.4 mg, 0.10 mmol) was added to a solution of ethyl 1H-pyrazol-1-ylacetate (8.0 mg, 0.052 mmol) (Key Organics/Bionet, Cat. #4Y-0601) in methanol (1.0 mL) and water (0.3 mL). The reaction mixture was stirred at r.t. overnight. The mixture was adjusted to pH=4 with aqueous HCl, and concentrated. The residue was dissolved in N,N-dimethylformamide (0.5 mL). To the solution was added 4-(4-methylpiperazin-1-yl)-6-(1,2,3,4-tetrahydroisoquinolin-7-yl)pyrimidin-2-amine HCl salt (15 mg, 0.034 mmol), followed by benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (18 mg, 0.041 mmol) and triethylamine (19 uL, 0.14 mmol). The reaction mixture was stirred at r.t. for 2 h. The mixture was purified by RP-LCMS (pH=10) to afford the desired product. Analytic LCMS (M+H)+: m/z=433.1.

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in N,N-dimethylformamide (0.5 mL)
3. stirringThe reaction mixture was stirred at r.t. for 2 h
4. customThe mixture was purified by RP-LCMS (pH=10)