反応 #3637

反応方程式

2-methylbenzoyl chloride

triethylamine

5,10-dihydro-5-(4-aminobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine

→

desired product

N-[4-(4H-Pyrazolo[5,1-c][1,4]benzodiazepin-5(10H)-ylcarbonyl)phenyl]-2-methylbenzamide

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄is then washed with water, 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 3 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 5 mmol of triethylamine and 3 mmol of 5,10-dihydro-5-(4-aminobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine. The mixture is stirred at room temperature for 5 hours and is then washed with water, 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, m.p. 142°-146° C.

出典