반응 #52191

반응 방정식

water

2-[2-(4-Amidinophenyl)-ethyl]-1-methyl-benzimidazole-5-yl-carboxylic acid-(4-benzamido-piperidinyl)-amide

Triethylamine

benzoyl chloride

→

2-[2-(4-Benzoylamidinophenyl)-ethyl]-1-methyl-benzimidazole-5-yl-carboxylic acid-(4-benzamidopiperidinyl)-amide

용매

dimethyl formamide

반응 조건

후처리

1. 1
   추출the aqueous phase is extracted with 20 ml of acetic ester
2. 2
   세척The organic phase is again washed with waterand
3. 3
   건조dried over sodium sulphate
4. 4
   workup.DISTILLATIONThe solvent is distilled off under vacuum
5. 5
   기타The residue is chromatographed over silica gel with acetic ester
6. 6
   기타the oily product is triturated with petroleum ether
7. 7
   여과The precipate is filtered
8. 8
   세척washed with petroleum ether
9. 9
   기타150-154° C.

실험 절차

1.0 g (2 mmol) of 2-[2-(4-Amidinophenyl)-ethyl]-1-methyl-benzimidazole-5-yl-carboxylic acid-(4-benzamido-piperidinyl)-amide and 3.2 ml Triethylamine (23 mmol) are dissolved in 10 ml of dimethyl formamide. The mixture is cooled down to 0° C. and 0.418 ml of benzoyl chloride (3.6 mmol) are slowly added dropwise. After 2 hours 20 ml of water are added to the mixture, and the aqueous phase is extracted with 20 ml of acetic ester. The organic phase is again washed with waterand dried over sodium sulphate. The solvent is distilled off under vacuum. The residue is chromatographed over silica gel with acetic ester, and the oily product is triturated with petroleum ether. The precipate is filtered and washed with petroleum ether. Yield: 0.160 g (15%); MPt: 150-154° C.;

출처