反应详情

5-Methyl-3-(trifluoromethyl)-1H-pyrazole-1-acetyl chloride (1.05 g, 2.5 mmol) (prepared as described in Example 19, step B) was dissolved in 10 mL of dichloromethane and added to a mixture of 2-(1-piperazinyl)-4-thiazolecarboxylate monohydrochloride (1.0 g, 3.0 mmol) (i.e. the product of Example 30, Step B) and powdered anhydrous potassium carbonate (2.2 g, 15.9 mmol) in 20 mL of dichloromethane at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 3 h. Then triethylamine (2 mL) was added to the reaction mixture, and the stirring was continued for an additional 30 minutes. The reaction mixture was diluted with dichloromethane, washed with 1 N aqueous hydrochloric acid, water, saturated aqueous solution of sodium bicarbonate and brine, and dried over magnesium sulfate. The filtered residue was evaporated in vacuo to give 1.0 g of a white foam. The resulting foam was slurried in 1-chlorobutane and filtered to give 0.83 g of the title compound as a white solid.

1. customat 0° C
2. waitthe stirring was continued for an additional 30 minutes
3. washwashed with 1 N aqueous hydrochloric acid, water, saturated aqueous solution of sodium bicarbonate and brine
4. dry with materialdried over magnesium sulfate
5. customThe filtered residue was evaporated in vacuo