反応 #3618

反応方程式

4-nitrobenzoyl chloride

10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine

triethylamine

→

desired product

10,11-Dihydro-10-(4-nitrobenzoyl)-5H-imidazo[2,1-c][1,4]benzodiazepine

溶媒

methylene chloride

ethyl acetate

methylene chloride

反応条件

後処理

1. 1
   その他followed by ice bath
2. 2
   温度cooling
3. 3
   workup.ADDITIONaddition
4. 4
   その他the ice bath is removed
5. 5
   その他The volatiles are removed in vacuo
6. 6
   その他to give a residue which
7. 7
   洗浄The solution is washed with water, and brine
8. 8
   乾燥The organic layer is dried with Na2SO4
9. 9
   ろ過filtered
10. 10
    その他evaporated in vacuo
11. 11
    その他to give a solid which
12. 12
    その他is purified by flash chromatography

実験手順

To a solution of 10 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 50 ml of methylene chloride under argon is added 15 mmol of triethylamine followed by ice bath cooling. A solution of 10 mmol of 4-nitrobenzoyl chloride in 10 ml of methylene chloride is added dropwise. Following complete addition, the ice bath is removed and the reaction mixture stirred at room temperature for 2 hours. The volatiles are removed in vacuo to give a residue which is dissolved in ethyl acetate. The solution is washed with water, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography to give desired product as a solid.

出典