反応 #3604

反応方程式

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

2,3-dimethylbenzoyl chloride

triethylamine

→

solid

収率 56.0%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,3-dimethylbenzamide

収率 56.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 5 hours
3. 3
   洗浄The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine
4. 4
   乾燥The reaction mixture is dried with Na2SO4
5. 5
   ろ過filtered
6. 6
   その他evaporated in vacuo
7. 7
   その他to give a solid which
8. 8
   その他is purified by flash chromatography

実験手順

To a stirred solution of 0.320 g of 2,3-dimethylbenzoyl chloride in 10 ml of methylene chloride is added 0.33 ml of triethylamine. After stirring for 15 minutes, 0.485 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 5 hours. The reaction mixture is washed with water, 1N HCl, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give 0.39 g of solid, m.p. 168°-170° C.

出典