反应详情

温度

0 °C

To a suspension of 240 mg (1.28 mmol) of 6-amino-quinoline-5-carboxylic acid in 9.60 mL of anhydrous tetrahydrofuran at 10° C., is added 372 mg (1.28 mmol) of 2-(3-chloro-pyridin-2-yl)-5-trifluoromethyl-2H-pyrazole-3-carboxylic acid followed by 5134 (6.38 mmol) of pyridine. Then the suspension is cooled to 0° C. and 398 μL (5.10 mmol) of methanesulfonyl chloride are added dropwise. The mixture is stirred at ambient temperature for 48 hours. Then the solvent is evaporated and the residue is precipitated with a minimum of ethyl acetate and washed with ethyl acetate. After filtration, water is added to the filtrate and the new suspension formed is filtrated again. After drying on high vacuum pump 303 mg (54%) of solid are obtained; LC/MS:444/446 (M+H)+.

1. customThen the solvent is evaporated
2. customthe residue is precipitated with a minimum of ethyl acetate
3. washwashed with ethyl acetate
4. filtrationAfter filtration, water
5. additionis added to the filtrate
6. customthe new suspension formed
7. filtrationis filtrated again
8. dry with materialAfter drying on high vacuum pump 303 mg (54%) of solid
9. customare obtained