반응 #3705

반응 방정식

NaOH

6,7-dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine

triethylamine

2,4-dichlorobenzoyl chloride

→

white solid

수율 99.2%

N-[4-[(6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-5-yl)carbonyl]-3-chlorophenyl]-2,4-dichlorobenzamide

수율 99.2%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타The volatiles are removed under vacuum and to the residue
2. 2
   workup.ADDITIONis added 2 ml of tetrahydrofuran and 1 ml of methanol
3. 3
   workup.STIRRINGThe mixture is stirred at room temperature for 2 hours
4. 4
   기타the volatiles removed
5. 5
   workup.ADDITIONTo the residue is added 2 ml of 1N NaOH and 5 ml of H2O
6. 6
   추출The mixture is extracted with ethyl acetate
7. 7
   세척the extract washed with brine
8. 8
   건조dried (Na2SO4)
9. 9
   기타The solvent is removed
10. 10
    기타the solid triturated with diethyl ether-hexane

실험 절차

To a mixture of 0.10 g of 6,7-dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine and 0.06 g of triethylamine in 6 ml of dichloromethane is added 0.10 g of 2,4-dichlorobenzoyl chloride in 0.5 ml of dichloromethane. The mixture is stirred at room temperature for 2 hours and 2 ml of 1N NaOH is added. The volatiles are removed under vacuum and to the residue is added 2 ml of tetrahydrofuran and 1 ml of methanol. The mixture is stirred at room temperature for 2 hours and the volatiles removed. To the residue is added 2 ml of 1N NaOH and 5 ml of H2O. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the solid triturated with diethyl ether-hexane to give 0.15 g of white solid, Mass Spectrum (CI): 510(M+H, Cl35).

출처