反応 #83509

反応方程式

(±)-2-chloro-2-phenylacetyl chloride

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

triethylamine

→

pink solid

収率 106.9%

α-Chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

収率 106.9%

溶媒

NaHCO3

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   その他The methylene chloride is evaporated
2. 2
   抽出the residue is extracted with ethyl acetate
3. 3
   洗浄The separated organic layer is washed with saturated NaHCO3 and brine
4. 4
   乾燥dried with Na2SO4
5. 5
   ろ過by filtering through a pad of hydrous magnesium silicate
6. 6
   その他The filtrate is evaporated to a residue which
7. 7
   workup.STIRRINGis stirred with etherhexane

実験手順

To a solution of 0.61 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 8 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.47 g of (±)-2-chloro-2-phenylacetyl chloride in 2 ml of methylene chloride. The mixture is stirred at room temperature for 1 hour and then diluted with 10 ml of 50% NaHCO3. The methylene chloride is evaporated and the residue is extracted with ethyl acetate. The separated organic layer is washed with saturated NaHCO3 and brine and then dried with Na2SO4 followed by filtering through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is stirred with etherhexane to give 0.98 g of pink solid. MS(CI): 456(M+H).

出典