تفاعل #83497

معادلة التفاعل

2-chlorobenzenesulfonyl chloride

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

triethylamine

→

white crystals

المردود 20.9%

10-[4-[[(2-Chlorophenyl)sulfonyl]amino]benzoyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

المردود 20.9%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   غسيلThe mixture is washed with 20 ml each of H2O, 2N citric acid, 1M NaHCO3, brine
2. 2
   تجفيفdried (Na2SO4)
3. 3
   ترشيحThe solution is filtered through a thin pad of hydrous magnesium silicate
4. 4
   تركيزthe filtrate concentrated to dryness
5. 5
   أخرىThe residue is chromatographed on thick layer silica gel plates (4) with the solvent ethyl acetate-hexane (1:1)
6. 6
   أخرىto give a solid
7. 7
   أخرىCrystallization from ethyl acetate

الإجراء التجريبي

To a solution of 0.418 g of 2-chlorobenzenesulfonyl chloride in 5 ml of dichloromethane, cooled to 0° C. is added 0.50 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine and 0.346 μl of triethylamine. The mixture is stirred at room temperature overnight and diluted with 50 ml of dichloromethane. The mixture is washed with 20 ml each of H2O, 2N citric acid, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated to dryness. The residue is chromatographed on thick layer silica gel plates (4) with the solvent ethyl acetate-hexane (1:1) to give a solid. Crystallization from ethyl acetate gives 0.165 g of white crystals, m.p. 206°-210° C.

المصدر