반응 #3603

반응 방정식

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

3-chlorobenzo[b]thiophen-2-carbonyl chloride

triethylamine

→

solid

수율 61.5%

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

수율 61.5%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 18 hours
3. 3
   세척The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine
4. 4
   건조The reaction mixture is dried with Na2SO4
5. 5
   여과filtered
6. 6
   기타evaporated in vacuo
7. 7
   기타to give a solid which
8. 8
   기타is purified by flash chromatography

실험 절차

To a stirred solution of 0.440 g of 3-chlorobenzo[b]thiophen-2-carbonyl chloride in 10 ml of methylene chloride is added 0.33 ml of triethylamine. After stirring for 15 minutes, 0.485 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 18 hours. The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give 0.49 g of solid, m.p. 220°-222° C.

출처