反応 #3652

反応方程式

2-methylbenzoyl chloride

triethylamine

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

→

desired product

N-[4-[(6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-5-yl)carbonyl)phenyl]-2-methyl-benzamide

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄The reaction mixture is washed with water, 2M citric acid, NaHCO3, and brine
2. 2
   乾燥The organic layer is dried with Na2SO4
3. 3
   ろ過filtered
4. 4
   その他evaporated in vacuo
5. 5
   その他to give a solid which
6. 6
   その他is purified by flash chromatography on silica gel

実験手順

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 6,7-dihydro-5-(4-aminobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine. The reaction mixture is washed with water, 2M 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; mass spectrum (CI): 422(M+H).

出典