反应 #3705

反应方程式

NaOH

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

triethylamine

2,4-dichlorobenzoyl chloride

→

white solid

收率 99.2%

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

收率 99.2%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   其他The 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
   其他the volatiles removed
5. 5
   workup.ADDITIONTo the residue is added 2 ml of 1N NaOH and 5 ml of H2O
6. 6
   萃取The mixture is extracted with ethyl acetate
7. 7
   洗涤the extract washed with brine
8. 8
   干燥dried (Na2SO4)
9. 9
   其他The solvent is removed
10. 10
    其他the solid triturated with diethyl ether-hexane

实验过程

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).

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