Triethylamine → HCID 46927538, compound

Participants

Reaction Steps

[Step 5] 36 mg (0.14 mmol) of the 1-(1-amino-3-methyl-2,3-dihydro-4,7-phenanthrolin-4(1H)-yl)ethanone, 51 mg (0.28 mmol) of copper (II) acetate, 43 mg (0.42 mmol) of triethylamine and 2 ml of a dichloromethane suspension containing 27 mg of molecular sieve (4A) were vigorously stirred for 18 hours. Following completion of the reaction, aqueous ammonium chloride solution was added followed by extraction with chloroform. The extract was washed with water and the organic layer was dehydrated with anhydrous sodium sulfate. The residue obtained by concentrating under reduced pressure was purified by silica gel column chromatography (ethyl acetate) and NH silica gel column chromatography (n-hexane:ethyl acetate=2:1) followed by crystallizing with diethyl ether and n-hexane to obtain 7 mg of the target compound in the form of a pale yellow crystalline powder (13%).

Provenance & Evidence