Reaktion #3687

Reaktionsgleichung

(±)-2-chloro-2-phenylacetyl chloride

10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

triethylamine

→

pink solid

Ausbeute 106.9%

α-Chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

Ausbeute 106.9%

Lösungsmittel

NaHCO3

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe methylene chloride is evaporated
2. 2
   Extraktionthe residue is extracted with ethyl acetate
3. 3
   WaschenThe separated organic layer is washed with saturated NaHCO3 and brine
4. 4
   Trocknendried with Na2SO4
5. 5
   Filtrationby filtering through a pad of hydrous magnesium silicate
6. 6
   SonstigeThe filtrate is evaporated to a residue which
7. 7
   workup.STIRRINGis stirred with ether-hexane

Vorschrift

To a solution of 0.61 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 8 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.47 g of (±)-2-chloro-2-phenylacetyl chloride in 2 ml of methylene chloride. The mixture is stirred at room temperature for 1 hour and then diluted with 10 ml of 50% NaHCO3. The methylene chloride is evaporated and the residue is extracted with ethyl acetate. The separated organic layer is washed with saturated NaHCO3 and brine and then dried with Na2SO4 followed by filtering through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is stirred with ether-hexane to give 0.98 g of pink solid. MS(CI): 456(M+H).

Quelle