Reaktion #3617

Reaktionsgleichung

10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine

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

triethylamine

→

desired product

N-[4-(5H-imidazo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2-methylbenzamide

Lösungsmittel

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe cooling bath is removed and after about 30 minutes a complete solution
2. 2
   Sonstigeis obtained
3. 3
   workup.STIRRINGto stir at room temperature for 1 hour
4. 4
   Einengenthe volatiles are concentrated in vacuo
5. 5
   workup.DISSOLUTIONThe residue is dissolved in 100 ml of ethyl acetate
6. 6
   Waschenwashed with water, 2N citric acid, and brine
7. 7
   SonstigeThe solution is dried with Na2 SO4
8. 8
   Einengenthe volatiles concentrated in vacuo

Vorschrift

To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 15 ml of methylene chloride, cooled to 0° C. is added 1.5 ml of triethylamine. After stirring for 3 minutes, 5 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 5 ml of methylene chloride is added. The cooling bath is removed and after about 30 minutes a complete solution is obtained. The reaction mixture is allowed to stir at room temperature for 1 hour and the volatiles are concentrated in vacuo. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, and brine. The solution is dried with Na2 SO4 and the volatiles concentrated in vacuo to give the desired product as a solid.

Quelle