反应详情

温度

80 °C

209 mg (0.67 mmol) of 4-fluoro-3-chlorophenylthiourea and 89 mg (0.70 mmol) of 1,3-dichloroacetone are dissolved in 5 ml of DMF, and the reaction solution is stirred at 80° C. for 3 h. After cooling, 209 mg (0.67 mmol) of the compound from example 2A and 224 mg (2.67 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 sat. sodium bicarbonate solution (5 ml) is added to the filtrate. The aqueous phase is extracted with ethyl acetate (three times, 5 ml each). The combined organic phases are dried over sodium 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. additionsat. sodium bicarbonate solution (5 ml) is added to the filtrate
6. extractionThe aqueous phase is extracted with ethyl acetate (three times, 5 ml each)
7. dry with materialThe combined organic phases are dried over sodium sulphate
8. customthe solvent is removed on a rotary evaporator