반응 #3582

반응 방정식

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

2,3-difluorobenzoyl chloride

triethylamine

→

solid

수율 13.7%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,3-difluorobenzamide

수율 13.7%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 72 hours
3. 3
   여과The reaction mixture is filtered
4. 4
   세척the solid washed with methylene chloride
5. 5
   세척The combined filtrate is washed with water, 2N citric acid, 1M NaHCO3, and brine
6. 6
   기타The reaction mixture is dried with Na2 SO4
7. 7
   여과filtered
8. 8
   기타evaporated in vacuo

실험 절차

To a stirred solution of 0.350 g of 2,3-difluorobenzoyl chloride in 5 ml of methylene chloride is added 0.346 ml of triethylamine. After stirring for 3 minutes, 0.500 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 72 hours. The reaction mixture is filtered and the solid washed with methylene chloride. The solid is saved. The combined filtrate is washed with water, 2N citric acid, 1M NaHCO3, and brine. The reaction mixture is dried with Na2 SO4, filtered and evaporated in vacuo to give 100 mg of a solid. The two solids are combined and dried to afford 790 mg of the desired product as a solid, m.p. 252°-258° C.

출처