反应详情

To a solution of 3-methyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine (7.9 mg, 0.053 mmol) in N,N-dimethylformamide (0.6 mL) was added sodium hydride (60%, 2.5 mg, 0.11 mmol) at 0° C. and the mixture was stirred at room temperature for 10 minutes. To the mixture was added a solution of tert-butyl 3-[3-chloro-5-(1-chloroethyl)-2-fluoro-6-methoxyphenyl]azetidine-1-carboxylate (20 mg, 0.053 mmol) in N,N-dimethylformamide (0.3 mL). The reaction mixture was stirred at 35° C. overnight, then quenched with water, extracted with ether. The combined organic layers were dried over MgSO4 and concentrated to afford the desired product which was used in next step directly. LCMS calculated for C23H29ClFN6O3 (M+H)+: m/z=491.2; Found: 491.1.

1. stirringThe reaction mixture was stirred at 35° C. overnight
2. customquenched with water
3. extractionextracted with ether
4. dry with materialThe combined organic layers were dried over MgSO4
5. concentrationconcentrated