4-methyloxolan-2-one

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 process is carried out as in Examples 1 - 5 using 50.0 grams of a methanolic co-distillate (boiling range 66° - 78° C) containing 14.8 grams of 2-methoxy-4-methyltetrahydrofuran derived from methallyl alcohol as described in step (a), 30 ml of water and 5.0 grams of powdered copper chromite (Catalysts and Chemicals Co.). The mixture is heated at 180° C under 1000 psi of hydrogen for one hour. Analysis of the product mixture shows the presence of 9.3 grams of 2-methyl-1,4-butandiol (70% yield) and about 0.5 grams of 3-methyl-4-butyrolactone (4% yield).

反応条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Methyl-dihydro-furan-2-one (4 g, 39.95 mmol) was dissolved in MeOH (10 ml) and the solution was cooled to −10° C. Thionyl chloride (3.6 ml, 49.9 mmol) was added dropwise. The mixture was stirred at −10° C. for 2 hrs and hereafter for 16 hrs at room temperature. The mixture was concentrated in vacuo to give crude 4-Chloro-3-methyl-butyric acid methyl ester (4 g, 87%) which was used in the next step without further purification. The mixture was concentrated in vacuo

反応条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Methyl-dihydro-furan-2-one (4 g, 39.95 mmol) was dissolved in MeOH (10 ml) and the solution was cooled to −10° C. Thionyl chloride (3.6 ml, 49.9 mmol) was added dropwise. The mixture was stirred at −10° C. for 2 hrs and hereafter for 16 hrs at room temperature. The mixture was concentrated in vacuo to give crude 4-Chloro-3-methyl-butyric acid methyl ester (4 g, 87%) which was used in the next step without further purification. The mixture was concentrated in vacuo

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

実験手順: The process is carried out as in Examples 1 - 5 using 50.0 grams of a methanolic co-distillate (boiling range 66° - 78° C) containing 14.8 grams of 2-methoxy-4-methyltetrahydrofuran derived from methallyl alcohol as described in step (a), 30 ml of water and 5.0 grams of powdered copper chromite (Catalysts and Chemicals Co.). The mixture is heated at 180° C under 1000 psi of hydrogen for one hour. Analysis of the product mixture shows the presence of 9.3 grams of 2-methyl-1,4-butandiol (70% yield) and about 0.5 grams of 3-methyl-4-butyrolactone (4% yield).

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

実験手順: The process is carried out as in Examples 1 - 5 using 50.0 grams of a methanolic co-distillate (boiling range 66° - 78° C) containing 14.8 grams of 2-methoxy-4-methyltetrahydrofuran derived from methallyl alcohol as described in step (a), 30 ml of water and 5.0 grams of powdered copper chromite (Catalysts and Chemicals Co.). The mixture is heated at 180° C under 1000 psi of hydrogen for one hour. Analysis of the product mixture shows the presence of 9.3 grams of 2-methyl-1,4-butandiol (70% yield) and about 0.5 grams of 3-methyl-4-butyrolactone (4% yield).

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Methyl-dihydro-furan-2-one (4 g, 39.95 mmol) was dissolved in MeOH (10 ml) and the solution was cooled to −10° C. Thionyl chloride (3.6 ml, 49.9 mmol) was added dropwise. The mixture was stirred at −10° C. for 2 hrs and hereafter for 16 hrs at room temperature. The mixture was concentrated in vacuo to give crude 4-Chloro-3-methyl-butyric acid methyl ester (4 g, 87%) which was used in the next step without further purification. The mixture was concentrated in vacuo

反応条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Methyl-dihydro-furan-2-one (4 g, 39.95 mmol) was dissolved in MeOH (10 ml) and the solution was cooled to −10° C. Thionyl chloride (3.6 ml, 49.9 mmol) was added dropwise. The mixture was stirred at −10° C. for 2 hrs and hereafter for 16 hrs at room temperature. The mixture was concentrated in vacuo to give crude 4-Chloro-3-methyl-butyric acid methyl ester (4 g, 87%) which was used in the next step without further purification. The mixture was concentrated in vacuo

反応条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Methyl-dihydro-furan-2-one (4 g, 39.95 mmol) was dissolved in MeOH (10 ml) and the solution was cooled to −10° C. Thionyl chloride (3.6 ml, 49.9 mmol) was added dropwise. The mixture was stirred at −10° C. for 2 hrs and hereafter for 16 hrs at room temperature. The mixture was concentrated in vacuo to give crude 4-Chloro-3-methyl-butyric acid methyl ester (4 g, 87%) which was used in the next step without further purification. The mixture was concentrated in vacuo

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

実験手順: The process is carried out as in Examples 1 - 5 using 50.0 grams of a methanolic co-distillate (boiling range 66° - 78° C) containing 14.8 grams of 2-methoxy-4-methyltetrahydrofuran derived from methallyl alcohol as described in step (a), 30 ml of water and 5.0 grams of powdered copper chromite (Catalysts and Chemicals Co.). The mixture is heated at 180° C under 1000 psi of hydrogen for one hour. Analysis of the product mixture shows the presence of 9.3 grams of 2-methyl-1,4-butandiol (70% yield) and about 0.5 grams of 3-methyl-4-butyrolactone (4% yield).