1,3-dioxolane

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:

反応条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 5 L three-neck flask was fitted with mechanical stirrer, thermometer, 500 mL additional funnel and argon purged. 1,3-Dioxalane (140 mL, 2.00 mol) in anhydrous Et2O (800 mL) and 1.0 M ZnCl2/Et2O (7.5 mL, 0.007 mol) were added. A solution of acetyl chloride (157 mL, 2.20 mol) in Et2O (200 mL) was added dropwise through an additional funnel over 20 min. A cold water bath was used to maintain temperature between 19-27° C. throughout. Continue stirring without external cooling for 4 h, reaction self heating at 20-25° C. for about 1 h. A clear, colorless solution retained under argon overnight. Stood for 3 days and formed an orange solution. Strip Et2O on rotavap (water aspirator) until no more distilled at 35° C. bath. A quantitative yield of product 318 g (theoretical yield 306 g) was obtained. A 5 L three-neck flask was fitted with mechanical stirrer thermometer, 500 mL additional funnel and argon purged A cold water bath was used without external cooling for 4 h reaction self heating at 20-25° C. for about 1 h Stood for 3 days formed an orange solution Strip Et2O on rotavap (water aspirator) until no more distilled at 35° C. bath

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

実験手順: A mixture of Dioxolane (B-5)(1.62 g), tetraethylammonium fluoride dihydrate (1.38 g) and acetic acid (0.5 ml) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The reaction mixture is diluted with ethyl acetate (50 ml), washed with saturated saline, dried and concentrated. The residue purified by silica gel chromatography to give tilted Lactam (C-5)(895 mg) from the fractions eluted with benzene-ethyl acetate (1:5). washed with saturated saline dried concentrated The residue purified by silica gel chromatography to give eluted with benzene-ethyl acetate (1:5)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 30.0 g of acetophenone are mixed with 24.5 g of dimethylamine hydrochloride and 74.1 g of 1,3-dioxolane, 2.5 g of concentrated hydrochloric acid are added, and the mixture is heated to exactly 90° C. and maintained at that temperature for 3.5 hours. Excess dioxolane is distilled off and the residue is cooled to 0° C. The resulting 3-dimethylamino-1-phenylpropan-1-one of formula are added the mixture is heated to exactly 90° C. maintained at that temperature for 3.5 hours Excess dioxolane is distilled off

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: 10.0 g of 2-thiopheneethanol, 11.5 g of 1,3-dioxolane, and 862 mg of indium(III) chloride were added to 780 mL of acetonitrile, and the resulting mixture was refluxed for 10 hours. The reaction product solution was cooled to room temperature and concentrated by evaporation under reduced pressure. To the residue, 100 mL of water and 150 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. The organic layer was separated and dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 6.6 g (yield of 60%) of the title compound, of which analysis data were the same as obtained in Example 14. the resulting mixture was refluxed for 10 hours concentrated by evaporation under reduced pressure To the residue, 100 mL of water and 150 mL of n-hexane were added The organic layer was separated dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was distilled under reduced pressure

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

実験手順: 10.0 g of 2-thiopheneethanol, 11.5 g of 1,3-dioxolane, and 862 mg of indium(III) chloride were added to 780 mL of acetonitrile, and the resulting mixture was refluxed for 10 hours. The reaction product solution was cooled to room temperature and concentrated by evaporation under reduced pressure. To the residue, 100 mL of water and 150 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. The organic layer was separated and dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 6.6 g (yield of 60%) of the title compound, of which analysis data were the same as obtained in Example 14. the resulting mixture was refluxed for 10 hours concentrated by evaporation under reduced pressure To the residue, 100 mL of water and 150 mL of n-hexane were added The organic layer was separated dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was distilled under reduced pressure