反応 #3582

反応方程式

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

2,3-difluorobenzoyl chloride

triethylamine

→

solid

収率 13.7%

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

収率 13.7%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 72 hours
3. 3
   ろ過The reaction mixture is filtered
4. 4
   洗浄the solid washed with methylene chloride
5. 5
   洗浄The combined filtrate is washed with water, 2N citric acid, 1M NaHCO3, and brine
6. 6
   その他The reaction mixture is dried with Na2 SO4
7. 7
   ろ過filtered
8. 8
   その他evaporated in vacuo

実験手順

To a stirred solution of 0.350 g of 2,3-difluorobenzoyl chloride in 5 ml of methylene chloride is added 0.346 ml of triethylamine. After stirring for 3 minutes, 0.500 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 72 hours. The reaction mixture is filtered and the solid washed with methylene chloride. The solid is saved. The combined filtrate is washed with water, 2N citric acid, 1M NaHCO3, and brine. The reaction mixture is dried with Na2 SO4, filtered and evaporated in vacuo to give 100 mg of a solid. The two solids are combined and dried to afford 790 mg of the desired product as a solid, m.p. 252°-258° C.

出典