反应详情

1-Amino-cyclohexanecarboxylic acid cyanomethyl-amide (1.0 mmol), [4-(2-methoxy-ethyl)-piperazin-1-yl]-benzoic acid hydrochloride (1.0 mmol), HOBT (1.0 mmol), WSCD (1.0 mmol) and triethylamine (1.0 mmol) are dissolved in DMF (4 ml) and stirred overnight at rt. After evaporation of the solvent, the residue is dissolved in a mixture of water and sodium carbonate (to ensure slightly basic conditions) and extracted three times with ethyl acetate. The combined extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with CH2Cl2/MeOH=92.5:7.5 as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether and the solid filtered of and dried (vacuum). A pale powder with mp. 166-168° C., Rf=0.37 (CH2Cl2/MeOH=9:1) is obtained.

1. customAfter evaporation of the solvent
2. dissolutionthe residue is dissolved in a mixture of water and sodium carbonate (
3. extractionextracted three times with ethyl acetate
4. extractionThe combined extract
5. dry with materialis dried over sodium sulfate
6. customevaporated
7. customThe residue is purified by flash chromatography on silica gel with CH2Cl2/MeOH=92.5:7.5 as mobile phase
8. additionThe product containing fractions
9. customevaporated
10. filtrationthe solid filtered of and
11. customdried (vacuum)
12. customA pale powder with mp. 166-168° C., Rf=0.37 (CH2Cl2/MeOH=9:1) is obtained