2-Methyl-1,3-dioxolane-2-ethanol

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

実験手順: The same procedure as in the steps (4f) to (4j) of Example 4 (a reprecipitation operation was not performed in oxidation step with 3-chloroperbenzoic acid) was repeated using 2-(2-methyl-1,3-dioxolan-2-yl)ethanol obtained in the step (69b) to obtain the title compound (410 mg, total 14.4% yield) as a light yellow solid. obtained in the step (69b)

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: The same procedure as in the steps (4f) to (4j) of Example 4 (a reprecipitation operation was not performed in oxidation step with 3-chloroperbenzoic acid) was repeated using 2-(2-methyl-1,3-dioxolan-2-yl)ethanol obtained in the step (69b) to obtain the title compound (410 mg, total 14.4% yield) as a light yellow solid. obtained in the step (69b)

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: The same procedure as in the steps (4f) to (4j) of Example 4 (a reprecipitation operation was not performed in oxidation step with 3-chloroperbenzoic acid) was repeated using 2-(2-methyl-1,3-dioxolan-2-yl)ethanol obtained in the step (69b) to obtain the title compound (410 mg, total 14.4% yield) as a light yellow solid. obtained in the step (69b)

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

実験手順: Lithium aluminium hydride (2 g, 51 mmol) is added in small portions to anhydrous ethyl ether (200 cc). The mixture is cooled to 0° C. and ethyl 3,3-ethylenedioxybutanoate (3 g, 17 mmol) is then added over 10 minutes as a solution in anhydrous ethyl ether (10 cc). The mixture is stirred for 2 hours 30 minutes at a temperature in the region of 20° C. and is then hydrolysed by adding a saturated sodium sulphate solution (12 cc). After 2 hours the white precipitate is separated off by filtration. The organic phases are dried over magnesium sulphate. 2,2-Ethylenedioxy-4-hydroxybutane (2.22 g) is thus obtained. After 2 hours the white precipitate is separated off by filtration The organic phases are dried over magnesium sulphate

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

実験手順: Lithium aluminium hydride (2 g, 51 mmol) is added in small portions to anhydrous ethyl ether (200 cc). The mixture is cooled to 0° C. and ethyl 3,3-ethylenedioxybutanoate (3 g, 17 mmol) is then added over 10 minutes as a solution in anhydrous ethyl ether (10 cc). The mixture is stirred for 2 hours 30 minutes at a temperature in the region of 20° C. and is then hydrolysed by adding a saturated sodium sulphate solution (12 cc). After 2 hours the white precipitate is separated off by filtration. The organic phases are dried over magnesium sulphate. 2,2-Ethylenedioxy-4-hydroxybutane (2.22 g) is thus obtained. After 2 hours the white precipitate is separated off by filtration The organic phases are dried over magnesium sulphate

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Pyridine (7.2 g) and chromic oxide (CrO3) (4.6 g) are added in small fractions to dichloromethane (150 cc) over 10 minutes. After 15 minutes' stirring at a temperature in the region of 20° C., 2,2-ethylenedioxy-4-hydroxybutane (0.85 g, 6.4 mmol) is added quickly as a solution in dichloromethane (2 cc). After 15 minutes' stirring at 20° C., the black, viscous precipitate is separated off by filtration through silica and is washed with ether. After evaporation of the solvents, 3,3-ethylenedioxybutanal (0.59 g) is obtained (B.P.0.4 =35° C.). the black, viscous precipitate is separated off by filtration through silica is washed with ether After evaporation of the solvents

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Pyridine (7.2 g) and chromic oxide (CrO3) (4.6 g) are added in small fractions to dichloromethane (150 cc) over 10 minutes. After 15 minutes' stirring at a temperature in the region of 20° C., 2,2-ethylenedioxy-4-hydroxybutane (0.85 g, 6.4 mmol) is added quickly as a solution in dichloromethane (2 cc). After 15 minutes' stirring at 20° C., the black, viscous precipitate is separated off by filtration through silica and is washed with ether. After evaporation of the solvents, 3,3-ethylenedioxybutanal (0.59 g) is obtained (B.P.0.4 =35° C.). the black, viscous precipitate is separated off by filtration through silica is washed with ether After evaporation of the solvents

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

実験手順: The same procedure as in the steps (4f) to (4j) of Example 4 (a reprecipitation operation was not performed in oxidation step with 3-chloroperbenzoic acid) was repeated using 2-(2-methyl-1,3-dioxolan-2-yl)ethanol obtained in the step (69b) to obtain the title compound (410 mg, total 14.4% yield) as a light yellow solid. obtained in the step (69b)