反応 #3647

反応方程式

2-methylbenzoyl chloride

triethylamine

4,10-dihydro-4-(4-aminobenzoyl)-5H-pyrrolo-[1,2-a]thieno[3,2-e][1,4]diazepine

→

desired product

N-[4-(5H-Pyrrolo[1,2-a]thieno[3,2-e][1,4]diazepin-4(10H)-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 reaction mixture 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 3 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 5 mmol of triethylamine and 3 mmol of 4,10-dihydro-4-(4-aminobenzoyl)-5H-pyrrolo-[1,2-a]thieno[3,2-e][1,4]diazepine. The mixture is stirred for 5 hours. The reaction mixture is washed with water, 2N citric acid, 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 on silica gel to give the desired product as a solid, m.p. 162°-188° C. (amorphous)

出典