反应详情

1.30 g of dicyclohexylcarbodiimide dissolved in 6 ml of dimethylformamide are added dropwise at 0° to 1.0 g of (R/S)-2-(3-hydroxy-2-oxo-1-pyrrolidinyl)acetic acid and 1.03 g of 94.7% cis-2-(2,6-dimethyl-1-piperidinyl)ethylamine dissolved in 20 ml of dimethylformamide. The mixture is left to stirred at room temperature for 4 days, treated with 0.23 of ion-free water and evaporated in a water-jet vacuum. The residue is treated five times with toluene and is each case again evaporated. The constituents of the residue which are soluble in chloroform are chromatographed on 60 g of aluminum oxide (activity grade III, neutral). The alcohol eluate is again chromatographed on 15 g of aluminum oxide (activity grade III, neutral). The fractions which are eluted with acetonitrile and ethanol contain, according to the gas chromatogram and mass spectrum, (R/S)-cis-N-[2-(2,6-dimethyl-1-piperidinyl)ethyl]-2-(3-hydroxy-2-oxo-1-pyrrolidinyl)acetamide.

1. waitThe mixture is left
2. customevaporated in a water-jet vacuum
3. additionThe residue is treated five times with toluene
4. customagain evaporated
5. customare chromatographed on 60 g of aluminum oxide (activity grade III, neutral)
6. customThe alcohol eluate is again chromatographed on 15 g of aluminum oxide (activity grade III, neutral)
7. washThe fractions which are eluted with acetonitrile and ethanol