تفاعل #3633

معادلة التفاعل

4-[(2-methylbenzoyl)amino]benzoyl chloride

triethylamine

5,10-dihydro-4H-pyrazolo[5,1-c][1,4]benzodiazepine

→

desired product

N-[4-(4H-Pyrazolo[5,1,c][1,4]benzodiazepin-5(10H)-ylcarbonyl)phenyl]-2-methylbenzamide

المذيبات

methylene chloride

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىthe volatiles are removed in vacuo
2. 2
   أخرىto give a residue
3. 3
   غسيلwashed with water, 2N citric acid, aqueous NaHCO3 and brine
4. 4
   تجفيفThe solution is dried with Na2SO4
5. 5
   أخرىthe solvent removed in vacuo
6. 6
   أخرىThe residue is purified by flash chromatography on silica gel with ethyl acetate-hexane

الإجراء التجريبي

To a mixture of 1.37 g of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 15 ml of methylene chloride, cooled to 0° C. is added 1.5 ml of triethylamine. To the mixture is added 5 mmol of 5,10-dihydro-4H-pyrazolo[5,1-c][1,4]benzodiazepine. The reaction mixture is allowed to stir at room temperature for 48 hours and the volatiles are removed in vacuo to give a residue. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, aqueous NaHCO3 and brine. The solution is dried with Na2SO4 and the solvent removed in vacuo. The residue is purified by flash chromatography on silica gel with ethyl acetate-hexane to give the desired product, m.p. 142°-146° C.

المصدر