methyl 3-(2-methyl-1,3-dioxolan-2-yl)propanoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An acetonitrile solution (10 ml) containing 5.0 g of methyl 2-methyl-l,3-dioxolane-2-propionate was added dropwise to 10 ml of a DMF suspension containing 2.3 g of 60% sodium hydride, and stirred at room temperature for 4 hours. The reaction mixture was poured into ice water, acidified with a saturated citric acid solution and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2) to provide 3.0 g of 2-methyl-β-oxo-1,3-dioxolane-2-pentanenitrile as oil. extracted with ethyl acetate The organic layer was washed with water a saturated saline solution and concentrated under reduced pressure The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An acetonitrile solution (10 ml) containing 5.0 g of methyl 2-methyl-l,3-dioxolane-2-propionate was added dropwise to 10 ml of a DMF suspension containing 2.3 g of 60% sodium hydride, and stirred at room temperature for 4 hours. The reaction mixture was poured into ice water, acidified with a saturated citric acid solution and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2) to provide 3.0 g of 2-methyl-β-oxo-1,3-dioxolane-2-pentanenitrile as oil. extracted with ethyl acetate The organic layer was washed with water a saturated saline solution and concentrated under reduced pressure The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: An acetonitrile solution (10 ml) containing 5.0 g of methyl 2-methyl-l,3-dioxolane-2-propionate was added dropwise to 10 ml of a DMF suspension containing 2.3 g of 60% sodium hydride, and stirred at room temperature for 4 hours. The reaction mixture was poured into ice water, acidified with a saturated citric acid solution and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2) to provide 3.0 g of 2-methyl-β-oxo-1,3-dioxolane-2-pentanenitrile as oil. extracted with ethyl acetate The organic layer was washed with water a saturated saline solution and concentrated under reduced pressure The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2)