3-甲基-5-戊内酯

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

实验步骤: According to the prior art methods, production of β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol requires respective independent production facilities. On the contrary, the simultaneous production method can produce β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol simultaneously from 2-hydroxy-4-methyltetrahydropyran with a common reactor and under relatively mild conditions. According to this simultaneous production method, β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol are produced generally in a β-methyl-δ-valerolactone/3-methylpentane-1,5-diol mole ratio of about 70/30 to 15/85. Said simultaneous production on method can give β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol each in a satisfactory yield and in a yield ratio therebetween selected depending on the demands therefor.

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

实验步骤: According to the prior art methods, production of β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol requires respective independent production facilities. On the contrary, the simultaneous production method can produce β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol simultaneously from 2-hydroxy-4-methyltetrahydropyran with a common reactor and under relatively mild conditions. According to this simultaneous production method, β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol are produced generally in a β-methyl-δ-valerolactone/3-methylpentane-1,5-diol mole ratio of about 70/30 to 15/85. Said simultaneous production on method can give β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol each in a satisfactory yield and in a yield ratio therebetween selected depending on the demands therefor.

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

实验步骤: According to the prior art methods, production of β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol requires respective independent production facilities. On the contrary, the simultaneous production method can produce β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol simultaneously from 2-hydroxy-4-methyltetrahydropyran with a common reactor and under relatively mild conditions. According to this simultaneous production method, β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol are produced generally in a β-methyl-δ-valerolactone/3-methylpentane-1,5-diol mole ratio of about 70/30 to 15/85. Said simultaneous production on method can give β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol each in a satisfactory yield and in a yield ratio therebetween selected depending on the demands therefor.

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

实验步骤: A solution of β-methyl-δ-valerolactone (3.0 g) in anhydrous dichloromethane (30 ml), cooled to 0-5° C., was saturated with hydrogen bromide gas and the mixture was stirred for three days at room temperature. The mixture was diluted with dichloromethane (100 ml) and the resulting solution was washed with 10-% NaCl (3×30 ml). Next the solution was dried with anhydrous MgSO4 and the solvent was distilled under reduced pressure, Yield 4.6 g. NMR ˜100% pure product. the resulting solution was washed with 10-% NaCl (3×30 ml) Next the solution was dried with anhydrous MgSO4 the solvent was distilled under reduced pressure, Yield 4.6 g

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

实验步骤: A solution of 16.0 g. (0.14 mol) 4-methyl-3,4,5,6-tetrahydro-2-pyranone in 50 ml. anhydrous ethanol is saturated with hydrogen bromide gas at 0°-5° C., left to stand overnight, poured into water and extracted with diethyl ether. The combined ether extracts are dried over anhydrous sodium sulphate and evaporated and the residue is distilled in a vacuum to give 21.9 g. (70% of theory) of the desired product in the form of a colourless liquid; b.p. 85°-87° C./0.1 mm.; nD20 =1.4590. left extracted with diethyl ether The combined ether extracts are dried over anhydrous sodium sulphate evaporated the residue is distilled in a vacuum to give 21.9 g

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

实验步骤: A solution of 16.0 g. (0.14 mol) 4-methyl-3,4,5,6-tetrahydro-2-pyranone in 50 ml. anhydrous ethanol is saturated with hydrogen bromide gas at 0°-5° C., left to stand overnight, poured into water and extracted with diethyl ether. The combined ether extracts are dried over anhydrous sodium sulphate and evaporated and the residue is distilled in a vacuum to give 21.9 g. (70% of theory) of the desired product in the form of a colourless liquid; b.p. 85°-87° C./0.1 mm.; nD20 =1.4590. left extracted with diethyl ether The combined ether extracts are dried over anhydrous sodium sulphate evaporated the residue is distilled in a vacuum to give 21.9 g

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

实验步骤: A solution of β-methyl-δ-valerolactone (3.0 g) in anhydrous dichloromethane (30 ml), cooled to 0-5° C., was saturated with hydrogen bromide gas and the mixture was stirred for three days at room temperature. The mixture was diluted with dichloromethane (100 ml) and the resulting solution was washed with 10-% NaCl (3×30 ml). Next the solution was dried with anhydrous MgSO4 and the solvent was distilled under reduced pressure, Yield: 4.6 g. NMR 100% pure product. the resulting solution was washed with 10-% NaCl (3×30 ml) Next the solution was dried with anhydrous MgSO4 the solvent was distilled under reduced pressure, Yield: 4.6 g

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

实验步骤: A solution of β-methyl-δ-valerolactone (3.0 g) in anhydrous dichloromethane (30 ml), cooled to 0-5° C., was saturated with hydrogen bromide gas and the mixture was stirred for three days at room temperature. The mixture was diluted with dichloromethane (100 ml) and the resulting solution was washed with 10-% NaCl (3×30 ml). Next the solution was dried with anhydrous MgSO4 and the solvent was distilled under reduced pressure, Yield: 4.6 g. NMR ˜100% pure product. the resulting solution was washed with 10-% NaCl (3×30 ml) Next the solution was dried with anhydrous MgSO4 the solvent was distilled under reduced pressure, Yield: 4.6 g

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

实验步骤: According to the prior art methods, production of β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol requires respective independent production facilities. On the contrary, the simultaneous production method can produce β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol simultaneously from 2-hydroxy-4-methyltetrahydropyran with a common reactor and under relatively mild conditions. According to this simultaneous production method, β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol are produced generally in a β-methyl-δ-valerolactone/3-methylpentane-1,5-diol mole ratio of about 70/30 to 15/85. Said simultaneous production on method can give β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol each in a satisfactory yield and in a yield ratio therebetween selected depending on the demands therefor.

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

实验步骤: According to the prior art methods, production of β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol requires respective independent production facilities. On the contrary, the simultaneous production method can produce β-methyl-δ-valerolactone and 3-methylpentane-1,5-diol simultaneously from 2-hydroxy-4-methyltetrahydropyran with a common reactor and under relatively mild conditions. According to this simultaneous production method, β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol are produced generally in a β-methyl-δ-valerolactone/3-methylpentane-1,5-diol mole ratio of about 70/30 to 15/85. Said simultaneous production on method can give β-methyl-δ-valerolactone and 3-methylpentane- 1,5-diol each in a satisfactory yield and in a yield ratio therebetween selected depending on the demands therefor.

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

实验步骤: A solution of β-methyl-δ-valerolactone (3.0 g) in anhydrous dichloromethane (30 ml), cooled to 0-5° C., was saturated with hydrogen bromide gas and the mixture was stirred for three days at room temperature. The mixture was diluted with dichloromethane (100 ml) and the resulting solution was washed with 10-% NaCl (3×30 ml). Next the solution was dried with anhydrous MgSO4 and the solvent was distilled under reduced pressure, Yield 4.6 g. NMR ˜100% pure product. the resulting solution was washed with 10-% NaCl (3×30 ml) Next the solution was dried with anhydrous MgSO4 the solvent was distilled under reduced pressure, Yield 4.6 g

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

实验步骤: A solution of 16.0 g. (0.14 mol) 4-methyl-3,4,5,6-tetrahydro-2-pyranone in 50 ml. anhydrous ethanol is saturated with hydrogen bromide gas at 0°-5° C., left to stand overnight, poured into water and extracted with diethyl ether. The combined ether extracts are dried over anhydrous sodium sulphate and evaporated and the residue is distilled in a vacuum to give 21.9 g. (70% of theory) of the desired product in the form of a colourless liquid; b.p. 85°-87° C./0.1 mm.; nD20 =1.4590. left extracted with diethyl ether The combined ether extracts are dried over anhydrous sodium sulphate evaporated the residue is distilled in a vacuum to give 21.9 g