反应 #3529413
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08653109B2
反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. After cooling the mixture is stirred at RT for a further 20 h The mixture is then filtered through a paper filter 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 the solvent is removed on a rotary evaporator
来源 ID: ord-dab2dc9de9024257854fee9ff8b76989