Embodiment 1:
α-methylamino Propiophenone hydrochloride 10g is dissolved in the 40-50mL methyl alcohol (content is more than 99%), stirs adding 5.5g Na BH down 4The borane reducing agent sodium hydride can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 30min down, after reaction finishes, methyl alcohol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, vacuum-drying, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 7.5g, calculating reaction yield with α-methylamino Propiophenone is 93.8%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 93.5: 6.5.
Embodiment 2:
α-methylamino Propiophenone hydrochloride 20g is dissolved in the 100mL dehydrated alcohol, stirs adding KBH down 42g, the borane reducing agent potassium hydride KH can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 3h down, after reaction finishes, ethanol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, steam empty dry, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 15.3, calculating reaction yield with α-methylamino Propiophenone is 95.6%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 97.1: 2.9.
Embodiment 3:
α-methylamino Propiophenone hydrochloride 100g is dissolved in the 300mL methyl alcohol (content is more than 99%), stirs adding 9.9g KBH down 4The borane reducing agent sodium hydride can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 30min down, after reaction finishes, methyl alcohol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, steam empty dry, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 76.8g, calculating reaction yield with α-methylamino Propiophenone is 96.0%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 94.7: 5.3.
Embodiment 4:
20g (±) ephedrine (content is 97.1%) is dissolved in the hot dehydrated alcohol of 50mL, add resolving agent D-amygdalic acid (for 0.5 times of amount of ephedrine mol ratio) simultaneously, slowly heated solution is to limpid transparent, after stopping heating, make its naturally cooling (for improving its crystallization velocity the ethanolic soln placement, also can place cold water or refrigerator to make its crystallization), usually in 2h, can obtain the crystallization of the salt of amygdalic acid and sanedrine formation, filter, and with a small amount of cold washing with alcohol crystallization 2-3 time, get the crystallization 15.62g that D-amygdalic acid and sanedrine form, this crystalline melt point is 167-169 ℃ after measured, and is consistent with literature value.
Embodiment 5:
With the crystallization 15.62g of the D-amygdalic acid of above-mentioned experiment gained and sanedrine with 15% NaOH solution dissolving, ephedrine is free separates out, extract at twice with the 25mL extracted with diethyl ether, combining extraction liquid, concentrating under reduced pressure is sloughed ether, adds 20% hcl acidifying in the enriched material, and left-handed ephedrine hydrochloride crystallization is separated out, filtration, drying get left-handed ephedrine hydrochloride 8.62g.
α-methylamino Propiophenone hydrochloride 10g is dissolved in the 40-50mL methyl alcohol (content is more than 99%), stirs adding 5.5g Na BH down 4The borane reducing agent sodium hydride can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 30min down, after reaction finishes, methyl alcohol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, vacuum-drying, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 7.5g, calculating reaction yield with α-methylamino Propiophenone is 93.8%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 93.5: 6.5.
Embodiment 2:
α-methylamino Propiophenone hydrochloride 20g is dissolved in the 100mL dehydrated alcohol, stirs adding KBH down 42g, the borane reducing agent potassium hydride KH can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 3h down, after reaction finishes, ethanol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, steam empty dry, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 15.3, calculating reaction yield with α-methylamino Propiophenone is 95.6%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 97.1: 2.9.
Embodiment 3:
α-methylamino Propiophenone hydrochloride 100g is dissolved in the 300mL methyl alcohol (content is more than 99%), stirs adding 9.9g KBH down 4The borane reducing agent sodium hydride can slowly add in the time in 15-30min, not being higher than 30 ℃ with the control temperature of reaction system is advisable, add the back and continue to stir reaction 30min down, after reaction finishes, methyl alcohol is reclaimed in underpressure distillation, enriched material adds 10%NaOH solution makes its dissolving, transfer the pH value of solution value greater than 11, the free postprecipitation of ephedrine is separated out, and filters, steam empty dry, the mixture of (±) ephedrine and (±) pseudoephedrine amounts to 76.8g, calculating reaction yield with α-methylamino Propiophenone is 96.0%, through liquid-phase chromatographic analysis wherein the ratio of (±) ephedrine and (±) pseudoephedrine be 94.7: 5.3.
Embodiment 4:
20g (±) ephedrine (content is 97.1%) is dissolved in the hot dehydrated alcohol of 50mL, add resolving agent D-amygdalic acid (for 0.5 times of amount of ephedrine mol ratio) simultaneously, slowly heated solution is to limpid transparent, after stopping heating, make its naturally cooling (for improving its crystallization velocity the ethanolic soln placement, also can place cold water or refrigerator to make its crystallization), usually in 2h, can obtain the crystallization of the salt of amygdalic acid and sanedrine formation, filter, and with a small amount of cold washing with alcohol crystallization 2-3 time, get the crystallization 15.62g that D-amygdalic acid and sanedrine form, this crystalline melt point is 167-169 ℃ after measured, and is consistent with literature value.
Embodiment 5:
With the crystallization 15.62g of the D-amygdalic acid of above-mentioned experiment gained and sanedrine with 15% NaOH solution dissolving, ephedrine is free separates out, extract at twice with the 25mL extracted with diethyl ether, combining extraction liquid, concentrating under reduced pressure is sloughed ether, adds 20% hcl acidifying in the enriched material, and left-handed ephedrine hydrochloride crystallization is separated out, filtration, drying get left-handed ephedrine hydrochloride 8.62g.
