反应详情

Under anhydrous conditions, a solution of 1-(5-Chloro-2-methyl-phenyl)-3-(1,3,5-trimethyl-1H-pyrazol-4-yl)-thiourea (2.3 g, 7.5 mmol) produced in example 8 and methyl iodide (0.94 mL, 15 mmol) in 70 mL of acetone was stirred at ambient temperature for 64 hours. The reaction mixture was concentrated in vacuo and partitioned between CH2Cl2 and saturated aqueous NaHCO3 solution. The organic phase was washed with dilute Na2S2O3 and dried (Na2SO4). Removal of solvent and crystallization of the residue from Et2O provided 1.78 g of title compound as a white solid (74% of theory, m.p. 134-135° C.).

1. concentrationThe reaction mixture was concentrated in vacuo
2. custompartitioned between CH2Cl2 and saturated aqueous NaHCO3 solution
3. washThe organic phase was washed with dilute Na2S2O3
4. dry with materialdried (Na2SO4)
5. customRemoval of solvent and crystallization of the residue from Et2O