反应详情

In 70 ml of ethanol was dissolved 1.06 g (5 mmol) of (S,S)-1,2-diphenylethylenediamine. In a nitrogen atmosphere and at room temperature, 30 ml of an ethanol solution containing 2.32 g (10.5 mmol) of 2-formyl-(2,4,6-trimethylphenyl)-1,3-dioxobutane was added to the solution, which was stirred for 2 hours at room temperature. The reaction mixture was then heated to 50° C. and reaction took place in 2 hours. After the completion of reaction, the solvent was distilled off in vacuum, obtaining a crude product. The crude product was dissolved in dichloromethane/ether/hexane for recrystallization, obtaining 2.28 g (isolation yield 71%) of an optically active ligand (N,N'-bis[3-oxo-2-(2,4,6-trimethylbenzoyl)butylidene]-(1S,2S)-1,2-diphenylethylenediamine) as white crystals. The thus obtained optically active ligand was analyzed by 1H-NMR, IR, and elemental analysis and measured for melting point and specific rotatory power. The results are shown below.

1. additionwas added to the solution, which
2. temperatureThe reaction mixture was then heated to 50° C.
3. customreaction
4. customin 2 hours
5. customAfter the completion of reaction
6. distillationthe solvent was distilled off in vacuum
7. customobtaining a crude product