反应详情

Sixty % sodium hydride in oil (9.60 g) is suspended in N,N-dimethyacetamide (500 ml), to this mixture is added methyl trans-4-(4-chlorobutyrylamino)-cyclohexanecarboxylate (52.32 g) obtained in Reference Example 113(2) gradually under ice-cooling. The reaction solution is warmed to room temperature, stirred for 24 hours, and thereto are poured saturated aqueous ammonium chloride solution and ice-water, and the mixture is extracted with chloroform. The organic layer is washed with saturated brine, dried over magnesium sulfate and evaporated to remove the solvent under reduced pressure. The resulting residue is purified by silica gel column chromatography (eluent: ethyl acetate) and the obtained solid is suspended in n-hexane-diisopropyl ether. The resulting crystals are collected by filtration and dried to give methyl trans-4-(2-oxo-pyrrolidin-1-yl)cyclohexanecarboxylate (39.20 g).

1. temperaturecooling
2. extractionthe mixture is extracted with chloroform
3. washThe organic layer is washed with saturated brine
4. dry with materialdried over magnesium sulfate
5. customevaporated
6. customto remove the solvent under reduced pressure
7. customThe resulting residue is purified by silica gel column chromatography (eluent: ethyl acetate)
8. filtrationThe resulting crystals are collected by filtration
9. customdried