反应详情

A solution of 2,4-diaminobenzaldehyde (1.00 g, 7.34 mmol), 1-methyl-4-piperidinone (1.08 ml, 8.81 mmol) and 4N aqueous sodium hydroxide solution (11 ml) in ethanol (70 ml) was stirred at 60° C. for 16 hrs, and the solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate, washed with aqueous potassium carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The obtained crude product was purified by NH-silica gel chromatography (elute solvent; ethyl acetate) and treated with ethyl acetate-isopropyl ether (1:5) to give the title compound (666 mg) as a powder.

1. customthe solvent was evaporated under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with aqueous potassium carbonate solution and saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe obtained crude product
6. customwas purified by NH-silica gel chromatography (elute solvent; ethyl acetate)
7. additiontreated with ethyl acetate-isopropyl ether (1:5)