Reaktion #3628

Reaktionsgleichung

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

triethylamine

9,10-dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

→

desired product

N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]diazepin-10-(9H)-ylcarbonyl)phenyl]-2-methylbenzamide

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture is concentrated in vacuo
2. 2
   workup.DISSOLUTIONthe residue is dissolved in 100 ml of ethyl acetate
3. 3
   Waschenwashed with water, 2N citric acid, aqueous NaHCO3 and brine
4. 4
   TrocknenThe solution is dried with Na2SO4
5. 5
   Einengenthe volatiles concentrated in vacuo
6. 6
   Sonstigeto give a solid which
7. 7
   Sonstigeis purified by flash chromatography

Vorschrift

To a mixture of 1.1 mmol of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 10 ml of methylene chloride, cooled to 0° C. is added 1.5 mmol of triethylamine. To the mixture is added 1 mmol of 9,10-dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine and the mixture stirred at room temperature for 2 hours. The reaction mixture is concentrated in vacuo and 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 volatiles concentrated in vacuo to give a solid which is purified by flash chromatography to give the desired product.

Quelle