1,3-二氧戊环-2,2-二乙醇

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M−1-1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.6 g (12 mmol) of dimethyl 2,2′-(1,3-dioxolane-2,2-diyl)diacetate in 100 mL of dry THF was added 1.4 g (36 mmol) of LAH at 0° C. The reaction mixture was then refluxed for 1 h, was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL). The mixture was stirred overnight, filtered through celite. The residue was washed twice with THF (100 mL×2). The combined organic phase was evaporated. Chromatography on silica gel afforded 1.3 g (8.0 mmol, yield: 66%) of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol: MS (m/e): 163 (M+1)+. The reaction mixture was then refluxed for 1 h was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL) filtered through celite The residue was washed twice with THF (100 mL×2) The combined organic phase was evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M+1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M+1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.6 g (12 mmol) of dimethyl 2,2′-(1,3-dioxolane-2,2-diyl)diacetate in 100 mL of dry THF was added 1.4 g (36 mmol) of LAH at 0° C. The reaction mixture was then refluxed for 1 h, was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL). The mixture was stirred overnight, filtered through celite. The residue was washed twice with THF (100 mL×2). The combined organic phase was evaporated. Chromatography on silica gel afforded 1.3 g (8.0 mmol, yield: 66%) of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol: MS (m/e): 163 (M+1)+. The reaction mixture was then refluxed for 1 h was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL) filtered through celite The residue was washed twice with THF (100 mL×2) The combined organic phase was evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M+1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.6 g (12 mmol) of dimethyl 2,2′-(1,3-dioxolane-2,2-diyl)diacetate in 100 mL of dry THF was added 1.4 g (36 mmol) of LAH at 0° C. The reaction mixture was then refluxed for 1 h, was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL). The mixture was stirred overnight, filtered through celite. The residue was washed twice with THF (100 mL×2). The combined organic phase was evaporated. Chromatography on silica gel afforded 1.3 g (8.0 mmol, yield: 66%) of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol: MS (m/e): 163 (M+1)+. The reaction mixture was then refluxed for 1 h was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL) filtered through celite The residue was washed twice with THF (100 mL×2) The combined organic phase was evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M+1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.6 g (12 mmol) of dimethyl 2,2′-(1,3-dioxolane-2,2-diyl)diacetate in 100 mL of dry THF was added 1.4 g (36 mmol) of LAH at 0° C. The reaction mixture was then refluxed for 1 h, was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL). The mixture was stirred overnight, filtered through celite. The residue was washed twice with THF (100 mL×2). The combined organic phase was evaporated. Chromatography on silica gel afforded 1.3 g (8.0 mmol, yield: 66%) of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol: MS (m/e): 163 (M+1)+. The reaction mixture was then refluxed for 1 h was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL) filtered through celite The residue was washed twice with THF (100 mL×2) The combined organic phase was evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M−1-1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.6 g (12 mmol) of dimethyl 2,2′-(1,3-dioxolane-2,2-diyl)diacetate in 100 mL of dry THF was added 1.4 g (36 mmol) of LAH at 0° C. The reaction mixture was then refluxed for 1 h, was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL). The mixture was stirred overnight, filtered through celite. The residue was washed twice with THF (100 mL×2). The combined organic phase was evaporated. Chromatography on silica gel afforded 1.3 g (8.0 mmol, yield: 66%) of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol: MS (m/e): 163 (M+1)+. The reaction mixture was then refluxed for 1 h was quenched with 15% NaOH aqueous solution (3 mL) and water (3 mL) filtered through celite The residue was washed twice with THF (100 mL×2) The combined organic phase was evaporated

反应条件: temp:-40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2,2′-(1,3-dioxolane-2,2-diyl)diethanol (1.3 g, 8.0 mmol) in methylene chloride (100 mL) was added triethylamine (3.4 mL, 24 mmol) at room temperature. The solution was cooled down to −40° C. and then mesyl chloride (1.65 mL, 20 mmol) was added dropwise. The reaction mixture was stirred at −40° C. for 30 min, then warmed up to 0° C. gradually. The reaction was quenched with saturated aqueous NaHCO3 solution. The aqueous layer was extracted with methylene chloride. The combined organic extracts were washed with brine, dried over Na2SO4, then evaporated to afford the crude product, 1,3-dioxolane-2,2-diyldiethane-2,1-diyl dimethanesulfonate: MS (m/e): 319 (M+1)+. warmed up to 0° C. gradually The reaction was quenched with saturated aqueous NaHCO3 solution The aqueous layer was extracted with methylene chloride The combined organic extracts were washed with brine dried over Na2SO4 evaporated