반응 #3687

반응 방정식

(±)-2-chloro-2-phenylacetyl chloride

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

triethylamine

→

pink solid

수율 106.9%

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

수율 106.9%

용매

NaHCO3

methylene chloride

methylene chloride

반응 조건

후처리

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

실험 절차

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).

출처