反应详情

温度

50 °C

A suspension of ethyl 2-[(5,6,6a,7,8,9-hexahydro-6a-methyl-4H-2-phenalenyl)amino]pyrimidine-5-carboxylate (0.043 g) in ethanol (5 ml) was added with 20% aqueous sodium hydroxide (1 ml), and the mixture was stirred at 50° C. for 3 hours. The reaction mixture was left to cool and then made acidic with 2 N aqueous hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was washed successively with water and saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from ethanol-chloroform to obtain the title compound (0.029 g, yield: 74%) as colorless needles (melting point: >300° C.).

1. waitThe reaction mixture was left
2. temperatureto cool
3. extractionthe mixture was extracted with chloroform
4. washThe organic layer was washed successively with water and saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationThe organic layer was concentrated under reduced pressure
7. customthe resulting residue was recrystallized from ethanol-chloroform