反应 #52191

反应方程式

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

溶剂

dimethyl formamide

反应条件

后处理

1. 1
   萃取the aqueous phase is extracted with 20 ml of acetic ester
2. 2
   洗涤The organic phase is again washed with waterand
3. 3
   干燥dried over sodium sulphate
4. 4
   workup.DISTILLATIONThe solvent is distilled off under vacuum
5. 5
   其他The residue is chromatographed over silica gel with acetic ester
6. 6
   其他the oily product is triturated with petroleum ether
7. 7
   过滤The precipate is filtered
8. 8
   洗涤washed with petroleum ether
9. 9
   其他150-154° C.

实验过程

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.;

来源