反应详情

0.43 g (1.51 mmol) of the compound from Example 2A, 0.38 g (3.78 mmol) of cyanothioacetamide and 0.38 g (3.78 mmol) of 4-methylmorpholine are dissolved in 15 ml of ethanol, and the mixture is stirred under reflux for 6 h. After cooling, the reaction solution is concentrated using a rotary evaporator, and the residue is chromatographed on silica gel 60. After removal of by-products (mobile phase gradient cyclohexane→cyclohexane/ethyl acetate 1:1), the product fractions are eluted (mobile phase gradient ethyl acetate→ethyl acetate/methanol 20:1). This is followed by fine purification via preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).

1. temperatureunder reflux for 6 h
2. temperatureAfter cooling
3. concentrationthe reaction solution is concentrated
4. customa rotary evaporator
5. customthe residue is chromatographed on silica gel 60
6. customAfter removal of by-products (mobile phase gradient cyclohexane→cyclohexane/ethyl acetate 1:1)
7. washthe product fractions are eluted (mobile phase gradient ethyl acetate→ethyl acetate/methanol 20:1)
8. customThis is followed by fine purification via preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)