反应详情

温度

90 °C

0.4 g (1.51 mmol) of methyl 2-cyano-3-[(4-methyl-3-pyridinyl)amino]-3-(methylsulfanyl)-2-propenoate are dissolved with 0.29 g (1.67 mmol) of 2-cyclohexylethanamidine hydrochloride and 0.46 g (3.3 mmol) of potassium carbonate in 5 ml of DMF and heated at 90° C. for 7 days. After cooling and filtration, the product is purified by preparative HPLC (YMC Gel ODS-AQ S 5/15 μm; eluent A; water, eluent B: acetonitrile, gradient: 0 min 30% B, 5 min 30% B, 50 min 95% B) purified. 433 mg (88% of theory) of the product are obtained.

1. temperatureAfter cooling
2. filtrationfiltration
3. customthe product is purified by preparative HPLC (YMC Gel ODS-AQ S 5/15 μm; eluent A; water, eluent B: acetonitrile, gradient: 0 min 30% B, 5 min 30% B, 50 min 95% B)
4. custompurified
5. custom433 mg (88% of theory) of the product are obtained