تفاعل #2608

معادلة التفاعل

sodium hydroxide

potassium cyanate

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-methoxyphenyl)benzamide

sodium bicarbonate

→

title compound

المردود 48.4%

4-Ureido-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-methoxyphenyl)benzamide

المردود 48.4%

المذيبات

acetic acid water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with ethyl acetate
2. 2
   غسيلThe resulting organic layer was washed with water and saturated brine
3. 3
   تجفيفdried on anhydrous sodium sulfate
4. 4
   أخرىThereafter, the solvent was removed by evaporation
5. 5
   أخرىthe resulting residue was purified by a silica gel column chromatography (chloroform:methanol=10:1)
6. 6
   أخرىrecrystallized from ethyl acetate-ether

الإجراء التجريبي

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-methoxyphenyl)benzamide (237.2 mg, 0.50 mmol) was dissolved in acetic acid-water (1:2, 1.8 ml) to which was subsequently added dropwise an aqueous solution (0.5 ml) of potassium cyanate (81.1 mg, 0.90 mmol) After 3 hours of stirring at room temperature, the reaction solution was mixed with saturated sodium bicarbonate aqueous solution, alkanized with 10% sodium hydroxide aqueous solution and then extracted with ethyl acetate. The resulting organic layer was washed with water and saturated brine, and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by a silica gel column chromatography (chloroform:methanol=10:1) and recrystallized from ethyl acetate-ether to obtain 125.6 mg (48.4%) of the title compound in a colorless powder form.

المصدر