تفاعل #2514309
ord-3da5b57ddd6d48b8bdf695b0e894b226
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المعالجة
- 1أخرىThe resulting reaction mixture
- 2غسيلAfterwards the reaction mixture was washed with water
- 3تجفيفagain with water, dried over sodium sulfate
- 4ترشيحfiltered
- 5أخرىevaporated to dryness in a rotavapor
- 6أخرىThe resulting crude solid was crystallized from ethanol
- 7أخرىThe crystallized solid was removed via filtration
- 8تركيزthe mother liquors were concentrated
- 9أخرىto yield a second fraction of crystallized product
الإجراء التجريبي
Under nitrogen atmosphere N-aminopiperidine (0.6 mL, 5.6 mmoles) and triethylamine (4 mL) were dissolved in methylene chloride (25 mL). The resulting mixture was ice-cooled down to 0° C. and a solution of 5-(4-chlorophenyl-1-(2,4-dichlorophenyl)-4,5-dihydro-pyrazole-3carboxylic acid chloride obtained in step (c) in methylene chloride (15 mL) was added dropwise. The resulting reaction mixture was stirred at room temperature (approximately 25° C.) overnight. Afterwards the reaction mixture was washed with water, followed by a saturated aqueous solution of sodium bicarbonate, then again with water, dried over sodium sulfate, filtered and evaporated to dryness in a rotavapor. The resulting crude solid was crystallized from ethanol. The crystallized solid was removed via filtration and the mother liquors were concentrated to yield a second fraction of crystallized product. The two fractions were combined to give a total amount of 1.7 g (57% of theoretical yield) of N-piperidinyl-5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4,5-dihydropyrazole-3-carboxamide having a melting point of 183-186° C.