反应详情

温度

120 °C

To a microwaveable vial containing 0.300 g (0.0011 mmol) of N-(6-hydroxy-naphthalen-1-yl)-benzamide in 1.5 mL DMF and 1.5 mL pyridine, was added 0.858 g (0.0028 mmol) of 4-chloro-6-methoxy-7-(2-pyrrolidin-1-yl-ethoxy)-quinoline. Copper grind was added (5 mmol %) to the mixture, along with 0.158 g (0.0025 mmol) KOH pellets. The vial was heated in a microwave for 18 min at 120° C., (60 Watts of constant power, powermax, CEM). The mixture was diluted with CH2Cl2 and water, then transferred to a seperatory funnel. The organics were extracted 3× with CH2Cl2. Then combined all organics, dried over Na2SO4, filtered, and concentrated in-vacuo. The crude was purified by reverse-phase HPLC. A tan oil was collected, which was the titled product. MS (ESI pos. ion) m/z: 534 (M+H). Calc'd for C33H31N3O4−533.23.

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