反应详情

5-(2-Amino-6-chloropyrimidin-4-yl)-2,4-dimethylbenzoic acid tert-butyl ester (Compound 1-1) (5.0 g, 15.0 mmol) obtained in Example 1-1 was dissolved in N,N-dimethylformamide (125 ml), and then cesium carbonate (11.5 g, 150.0 mmol) and 2-aminoethanethiol (48.8 g, 150.0 mmol) were added thereto at room temperature. The resulting mixture was stirred at room temperature for three hours, and then diluted with ethyl acetate (500 ml). The solution was sequentially washed with water (500 ml, three times) and a saturated aqueous sodium chloride solution (500 ml). The washed organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The resulting crude product was dissolved in ethyl acetate (20 ml) while heating, and n-hexane (60 ml) was added thereto. The mixture was stirred at room temperature for one hour. The precipitated crystals were collected by filtration. After washing with n-hexane (60 ml), the crystals were dried under reduced pressure to yield 5-[2-amino-6-(2-aminoethylsulfanyl)pyrimidin-4-yl]-2,4-dimethylbenzoic acid tert-butyl ester (4.4 g) as colorless crystals.

1. customat room temperature
2. washThe solution was sequentially washed with water (500 ml, three times)
3. dry with materialThe washed organic layer was dried over anhydrous sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. dissolutionThe resulting crude product was dissolved in ethyl acetate (20 ml)
7. temperaturewhile heating
8. additionn-hexane (60 ml) was added
9. stirringThe mixture was stirred at room temperature for one hour
10. filtrationThe precipitated crystals were collected by filtration
11. washAfter washing with n-hexane (60 ml)
12. customthe crystals were dried under reduced pressure