Phenol → HCID 66872788, compound

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence