(2,2-Dimethyl-1,3-dioxolan-4-yl)methyl acetate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To a mixture of 4-hydroxymethyl-2,2-dimethyl-1,3-dioxolane (5.35 g) and pyridine (15.65 g) in dichloromethane (200 ml) was added acetic anhydride (20.56 g), and the mixture was stirred at ambient temperature for 12 hours. The mixture was poured into a mixture of water and ethyl acetate. The organic layer was separated, washed with saturated aqueous sodium hydrogen carbonate and brine successively, dried over magnesium sulfate, and evaporated in vacuo to give 4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (6.02 g). The organic layer was separated washed with saturated aqueous sodium hydrogen carbonate and brine successively dried over magnesium sulfate evaporated in vacuo

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

実験手順: To a mixture of 4-hydroxymethyl-2,2-dimethyl-1,3-dioxolane (5.35 g) and pyridine (15.65 g) in dichloromethane (200 ml) was added acetic anhydride (20.56 g), and the mixture was stirred at ambient temperature for 12 hours. The mixture was poured into a mixture of water and ethyl acetate. The organic layer was separated, washed with saturated aqueous sodium hydrogen carbonate and brine successively, dried over magnesium sulfate, and evaporated in vacuo to give 4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (6.02 g). The organic layer was separated washed with saturated aqueous sodium hydrogen carbonate and brine successively dried over magnesium sulfate evaporated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To a mixture of 4-hydroxymethyl-2,2-dimethyl-1,3-dioxolane (5.35 g) and pyridine (15.65 g) in dichloromethane (200 ml) was added acetic anhydride (20.56 g), and the mixture was stirred at ambient temperature for 12 hours. The mixture was poured into a mixture of water and ethyl acetate. The organic layer was separated, washed with saturated aqueous sodium hydrogen carbonate and brine successively, dried over magnesium sulfate, and evaporated in vacuo to give 4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (6.02 g). The organic layer was separated washed with saturated aqueous sodium hydrogen carbonate and brine successively dried over magnesium sulfate evaporated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Then sodium carbonate (40.63 g, 0.294 mol) was added to a mixture of 4-acetoxymethyl-2,2-dimethyl-1,3-dioxolane (34.18 g, 0.196 mol) and methanol (200 ml) and the resulting mixture was stirred for 8 hours at 25° C. After completion of the reaction the salt was filtered off and the filtrate was condensed in vacuo and water was added to the residue and extracted with methylene chloride. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and condensed in vacuo. The crude product was distilled to give 23.12 g of 2,2-dimethyl-1,3-dioxolane-4-methanol (yield 89%, b.p. 72° C. at 8 mmHg). After completion of the reaction the salt was filtered off condensed in vacuo and water was added to the residue extracted with methylene chloride The extract was washed with saturated brine dried over anhydrous sodium sulfate and condensed in vacuo The crude product was distilled