反応 #3678

反応方程式

NaOH

10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

triethylamine

diphenylphosphinyl chloride

→

white solid

収率 96.4%

10-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine

収率 96.4%

溶媒

dichloromethane

反応条件

後処理

1. 1
   抽出The mixture is extracted with ethyl acetate
2. 2
   洗浄the extract washed with brine
3. 3
   乾燥dried (Na2SO4)
4. 4
   その他The solvent is removed
5. 5
   その他the residue triturated with ether-hexane

実験手順

A mixture of 0.10 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine 0.060 g of triethylamine and 0.12 g of diphenylphosphinyl chloride in 2 ml of dichloromethane is stirred at room temperature for 2 hours and then 1N NaOH is added. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the residue triturated with ether-hexane to give 0.16 g of a white solid.

出典