反应详情

温度

180 °C

Phenol (21.4 mg), cesium carbonate (74.0 mg), copper(I) chloride (11.2 mg) and 2,2,6,6-tetramethylheptane-3,5-dione (2.1 mg) were added to an N-methylpyrrolidine (1.0 mL) solution of the compound (50.0 mg) obtained in Example 109 (Step 1), and with irradiation with microwaves, this was stirred at 180° C. for 20 minutes. The reaction liquid was diluted with ethyl acetate, and washed with water. The organic layer was dried with sodium sulfate, then filtered, and concentrated under reduced pressure. The residue was purified through reversed-phase HPLC (0.1% TFA acetonitrile/H2O=from 10% to 90%, gradient), and further purified through preparative thin-layer chromatography (NH silica gel, methanol/chloroform=10%) to give the entitled compound (4.0 mg, 8%) as a colorless oily substance.

1. customwith irradiation with microwaves
2. customThe reaction liquid
3. washwashed with water
4. dry with materialThe organic layer was dried with sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified through reversed-phase HPLC (0.1% TFA acetonitrile/H2O=from 10% to 90%, gradient)
8. customfurther purified through preparative thin-layer chromatography (NH silica gel, methanol/chloroform=10%)