反应详情

A suspension of sodium hydride (60%, 0.008 g) in N,N-dimethylformamide (2 ml) was added with ethyl 2-[(5,6,6a,7,8,9-hexahydro-6a-methyl-4H-2-phenalenyl)amino]pyrimidine-5-carboxylate (0.034 g) dissolved in N,N-dimethylformamide (1 ml), and the mixture was stirred at room temperature for 10 minutes. The reaction mixture was added with iodomethane (0.018 ml), and the mixture was stirred overnight. The reaction mixture was added with saturated aqueous ammonium chloride, and the mixture was extracted with diethyl ether. 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 suspended in ethanol (5 ml), the suspension 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 to obtain the title compound (0.028 g, yield: 85%) as colorless needles (melting point: >300° C.).

1. stirringthe mixture was stirred overnight
2. extractionthe mixture was extracted with diethyl ether
3. washThe organic layer was washed successively with water and saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationThe organic layer was concentrated under reduced pressure
6. additionthe suspension was added with 20% aqueous sodium hydroxide (1 ml)
7. stirringthe mixture was stirred at 50° C. for 3 hours
8. waitThe reaction mixture was left
9. temperatureto cool
10. extractionthe mixture was extracted with chloroform
11. washThe organic layer was washed successively with water and saturated brine
12. dry with materialdried over anhydrous sodium sulfate
13. concentrationThe organic layer was concentrated under reduced pressure
14. customthe resulting residue was recrystallized from ethanol