反应详情

N-Methyl-2-(4-acetylamino-2-isopropyl-5-methylphenoxy)ethylamine (4.94 g) and 2,5-dimethoxy-3,4,6-trimethylbenzyl chloride (4.29 g) were dissolved in N,N-dimethylformamide (70 ml), and triethylamine (1.89 g) was added dropwise while stirring the mixture at room temperature. The mixture was stirred at room temperature for 16.5 hours. After the reaction, the solvent was distilled off, and water was added. The mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained crude product was purified by silica gel chromatography (eluent; ethyl acetate/benzene=1/1) to give 6.40 g of a pale-yellow solid. A portion (1.0 g) was taken therefrom and recrystallized from diisopropyl ether to give 0.62 g of the title compound (colorless crystals).

1. stirringThe mixture was stirred at room temperature for 16.5 hours
2. customAfter the reaction
3. distillationthe solvent was distilled off
4. additionwater was added
5. extractionThe mixture was extracted with ethyl acetate
6. washThe obtained organic layer was washed with saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe obtained crude product
10. customwas purified by silica gel chromatography (eluent; ethyl acetate/benzene=1/1)