反応 #3589

反応方程式

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

2-fluorobenzoyl chloride

triethylamine

→

desired product

収率 88.4%

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

収率 88.4%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   その他The bath is removed
2. 2
   workup.STIRRINGthe reaction mixture stirred at room temperature for 18 hours
3. 3
   濃縮The volatiles are concentrated in vacuo
4. 4
   その他to give a residue which
5. 5
   洗浄washed with water, 2N citric acid, 1M NaHCO3 and brine
6. 6
   乾燥The organic layer is dried with Na2SO4
7. 7
   ろ過filtered
8. 8
   濃縮concentrated in vacuo

実験手順

To a solution of 314 mg of 2-fluorobenzoyl chloride in 5 ml of methylene chloride at 0° C. is added 346 μl of triethylamine. After stirring for 3 minutes, 500 mg of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added. The bath is removed and the reaction mixture stirred at room temperature for 18 hours. The volatiles are concentrated in vacuo to give a residue which is dissolved in methylene chloride, washed with water, 2N citric acid, 1M NaHCO3 and brine. The organic layer is dried with Na2SO4, filtered and concentrated in vacuo to give 620 mg of the desired product as a crystalline solid, m.p. 257°-260° C.

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