反応 #3642

反応方程式

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

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄The reaction mixture is washed with water, 2N 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 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.

出典