تفاعل #52191

معادلة التفاعل

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

المذيبات

dimethyl formamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe aqueous phase is extracted with 20 ml of acetic ester
2. 2
   غسيلThe organic phase is again washed with waterand
3. 3
   تجفيفdried over sodium sulphate
4. 4
   workup.DISTILLATIONThe solvent is distilled off under vacuum
5. 5
   أخرىThe residue is chromatographed over silica gel with acetic ester
6. 6
   أخرىthe oily product is triturated with petroleum ether
7. 7
   ترشيحThe precipate is filtered
8. 8
   غسيلwashed with petroleum ether
9. 9
   أخرى150-154° C.

الإجراء التجريبي

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.;

المصدر