反应详情

温度

80 °C

18 mg (0.10 mmol) of 4-fluorophenylthiourea and 13 mg (0.10 mmol) of 1,3-dichloroacetone are dissolved in 2 ml of DMF, and the reaction solution is stirred at 80° C. for 3 h. After cooling, 89 mg (0.09 mmol, 33% pure) of the compound from example 4A and 32 mg (0.38 mmol) of sodium bicarbonate are added, and the mixture is stirred at RT for a further 20 h. The mixture is then filtered through a paper filter, and the filtrate is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). Sat. sodium bicarbonate solution (5 ml) is added to the product fraction obtained, and the mixture is extracted with ethyl acetate (three times, 5 ml each). The combined organic phases are dried over magnesium sulphate, and the solvent is removed on a rotary evaporator.

1. temperatureAfter cooling
2. stirringthe mixture is stirred at RT for a further 20 h
3. filtrationThe mixture is then filtered through a paper
4. filtrationfilter
5. customthe filtrate is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
6. additionSat. sodium bicarbonate solution (5 ml) is added to the product fraction
7. customobtained
8. extractionthe mixture is extracted with ethyl acetate (three times, 5 ml each)
9. dry with materialThe combined organic phases are dried over magnesium sulphate
10. customthe solvent is removed on a rotary evaporator