反応 #3702

反応方程式

2-chloro-4-nitrobenzoyl chloride

6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine

triethylamine

→

yellow foam

収率 105.6%

6,7-Dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepin

収率 105.6%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   その他then quenched with 5 ml of saturated NaHCO3
2. 2
   その他The methylene chloride is evaporated in vacuo
3. 3
   workup.ADDITIONthe residue is diluted with 5 ml of water
4. 4
   抽出extracted with 20 ml of ethyl acetate
5. 5
   その他The organic layer is separated
6. 6
   洗浄washed with saturated NaHCO3 and brine
7. 7
   乾燥dried with Na2SO4
8. 8
   その他evaporated in vacuo

実験手順

To a solution of 0.28 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 6 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.50 g of 2-chloro-4-nitrobenzoyl chloride in 0.5 ml of methylene chloride. The reaction mixture is stirred at room temperature for 1 hour then quenched with 5 ml of saturated NaHCO3. The methylene chloride is evaporated in vacuo and the residue is diluted with 5 ml of water and extracted with 20 ml of ethyl acetate. The organic layer is separated washed with saturated NaHCO3 and brine, dried with Na2SO4 and evaporated in vacuo to give 0.59 g of a yellow foam which is triturated with ether-hexanes to give 0.56 g of the desired product as off-white solid. MS(CI): 368(M+H)(Cl35) 370 (M+H) (Cl37)

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