反应详情

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0 °C

A suspension containing 4.58 g of 2,4-diamino-6-[2-(4-tert-butoxycarbonylphenyl)prop-1-enyl]pyrido[2,3-d]pyrimidine in 200 mL of a saturated solution of hydrogen chloride gas in nitromethane was stirred at 0° C. for 1 hour, and then at room temperature for 3 hours. After dilution with ether, the reaction mixture was filtered and the collected solid was washed successively with water, methanol, and acetone and then dried under reduced pressure to give 3.90 g (100%) of 2,4-diamino-6-[2-(4-carboxyphenyl)prop-1-enyl]pyrido[2,3-d]pyrimidine. NMR (DMSO-d6, 80 MHz) d 2.31 (brs, 3H), 6.77 and 7.07 (brs, 1H), 7.74 (d, 2H, J=8.5 Hz), 7.98 (d, 2H, J=8.5 Hz), 8.26, (d, 1H, J=2.0 Hz), 8.74 d, 1H, J=2.0 Hz).

1. waitat room temperature for 3 hours
2. filtrationAfter dilution with ether, the reaction mixture was filtered
3. washthe collected solid was washed successively with water, methanol, and acetone
4. customdried under reduced pressure