反应详情

温度

120 °C

To a microwaveable vial containing 0.300 g (1.1 mmol) of N-(6-hydroxy-naphthalen-1-yl)-benzamide in 1.5 mL DMF and 1.5 mL pyridine, was added 0.771 g (2.8 mmol) of [2-(4-chloro-6-methoxy-quinolin-7-yloxy)-ethyl]-dimethylamine. Then added (5 mmol %) copper grind into the mixture, along with 0.158 g (2.5 mmol) KOH pellets. The vial was heated in a microwave for 18 min at 120° C. (60 Watts constant power, CEM powermax). The mixture was diluted with CH2Cl2 and water, then transferred to seperatory funnel. The organics were extracted 3× with CH2Cl2. The organic layers were combined, dried over Na2SO4, filtered, and concentrated in-vacuo. The crude was purified by reverse-phase HPLC. A tan oil was collected, which was titled product. MS (ESI pos. ion) m/z: 508 (M+H). Calc'd for C31H29N3O4−507.22.

1. customtransferred to seperatory funnel
2. extractionThe organics were extracted 3× with CH2Cl2
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in-vacuo
6. customThe crude was purified by reverse-phase HPLC
7. customA tan oil was collected