반응 #3642

반응 방정식

2-methylbenzoyl chloride

triethylamine

9,10-dihydro-10-(4-aminobenzoyl)-4H-pyrrolo-[1,2-a]thieno[2,3-e][1,4]diazepine

→

desired product

N-[4-(4H-Pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepin-10(9H)-ylcarbonyl)phenyl]-2-methylbenzamide

용매

methylene chloride

반응 조건

후처리

1. 1
   세척The reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine
2. 2
   건조The organic layer is dried with Na2SO4
3. 3
   여과filtered
4. 4
   기타evaporated in vacuo
5. 5
   기타to give a solid which
6. 6
   기타is purified by flash chromatography on silica gel

실험 절차

To a stirred solution of 5 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 7 mmol of triethylamine and 5 mmol of 9,10-dihydro-10-(4-aminobenzoyl)-4H-pyrrolo-[1,2-a]thieno[2,3-e][1,4]diazepine and the mixture stirred for 5 hours. The reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give the desired product as a solid.

출처