反应详情

To a solution of 4-(2-(3-iodophenoxyl)ethyl)morpholine (1.0 g, 2.9 mmol) in anhydrous toluene (20 mL) was added 3-isopropyl-1H-pyrazol-5-amine (397 mg, 3.17 mmol) followed by (1R,2R)—N1,N2-dimethylcyclohexane-1,2-diamine (227 μL, 1.44 mmol) and potassium carbonate (1.99 g, 14.4 mmol). The mixture was purged with N2, copper(I) iodide (82 mg, 0.43 mmol) was added and the reaction mixture was heated at reflux under N2 for 64 hr. The resulting mixture was cooled to RT and was partitioned between EtOAc and water (100 mL). The organic layer was separated and washed with brine (2×100 mL) and was then dried and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, 40 g, 0-20% MeOH in DCM, gradient elution) to afford the title compound, Intermediate A13, as a brown oil (325 mg, 33%); Rt 1.66 min (Method 2, basic); m/z 329 (M+H)+ (ES+).

1. additionwas added
2. temperaturethe reaction mixture was heated
3. temperatureat reflux under N2 for 64 hr
4. customwas partitioned between EtOAc and water (100 mL)
5. customThe organic layer was separated
6. washwashed with brine (2×100 mL)
7. customwas then dried
8. customevaporated in vacuo
9. customThe residue was purified by flash column chromatography (SiO2, 40 g, 0-20% MeOH in DCM, gradient elution)