反应详情

Add AlMe3 (1.72 mL, 3.44 mmol, 2M solution in hexane) to a solution of 2,2-dimethyl-propylamine (402 μL, 3.44 mmol) in DCM (0.5 mL) under nitrogen atmosphere. Stir the mixture for 15 min at room temperature and add ethyl 2-(4-cyanophenyl)propanoate. Heat the mixture at 40° C. overnight. Quench the reaction with 10N aqueous HCl and extract twice with DCM. Dry the combined organics extracts over Na2SO4, filter and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (7:3) to obtain the desired intermediate (170 mg, 41%).

1. temperatureHeat the mixture at 40° C. overnight
2. customQuench
3. customthe reaction with 10N aqueous HCl
4. extractionextract twice with DCM
5. customDry the combined
6. filtrationfilter
7. concentrationconcentrate in vacuo
8. customPurify by chromatography on silica gel eluting with hexane/EtOAc (7:3)