DL-α-氨基-ε-己内酰胺盐酸盐

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in 1,2-propanediol (1.2 L) is heated to reflux. A Dean-Stark trap is used to withdraw the first 120 mL of condensed solvent. The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which maybe determined by 1H NMR). The solution is cooled and is concentrated under vacuum. Ethanol is used to completely dissolve the α-amino-ε-caprolactam 2. Byproduct NaCl is removed by filtration. The filtrate is concentrated and the resulting crude α-amino-ε caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (36.5 g) in 74% yield. is heated to reflux to withdraw the first 120 mL of condensed solvent The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which The solution is cooled is concentrated under vacuum to completely dissolve the α-amino-ε-caprolactam 2 Byproduct NaCl is removed by filtration The filtrate is concentrated the resulting crude α-amino-ε caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in hexanol (1.2 L) is heated to reflux with a Dean-Stark trap used to remove H2O. The suspension is refluxed for 8 hours until all starting material is consumed (which maybe determined by 1H NMR). The suspension is then cooled and filtered to remove byproduct NaCl. The filtrate is concentrated and the resulting crude α-amino-ε-caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (37 g) in 75% yield. is heated to reflux with a Dean-Stark trap to remove H2O The suspension is refluxed for 8 hours until all starting material is consumed (which The suspension is then cooled filtered to remove byproduct NaCl The filtrate is concentrated the resulting crude α-amino-ε-caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature

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

实验步骤: The contents, taken out from the glass ampule, were neutralized to about pH 8.0 by adding sodium ethylate-ethanol solution, and the mixture of α-amino-ε-caprolactam hydrochloride, lysine ethyl ester monohydrochloride, and a small amount of lysine ethyl ester dihydrochloride, was obtained. α-amino-ε-caprolactam hydrochloride, lysine ethyl ester dihydrochloride, and sodium chloride were eluted by passing the mixture through the weak cation exchange column, Amberlite IRC-50, freed from water before use, and washing the column with ethanol. Then, 1.18 grs. of lysine ethyl ester monohydrochloride was eluted in the form of the dihydrochloride salt by charging ethanolic hydrochloride into the weak cation exchange column. (yield 40%)

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

实验步骤: The contents, taken out from the glass ampule, were neutralized to about pH 8.0 by adding sodium ethylate-ethanol solution, and the mixture of α-amino-ε-caprolactam hydrochloride, lysine ethyl ester monohydrochloride, and a small amount of lysine ethyl ester dihydrochloride, was obtained. α-amino-ε-caprolactam hydrochloride, lysine ethyl ester dihydrochloride, and sodium chloride were eluted by passing the mixture through the weak cation exchange column, Amberlite IRC-50, freed from water before use, and washing the column with ethanol. Then, 1.18 grs. of lysine ethyl ester monohydrochloride was eluted in the form of the dihydrochloride salt by charging ethanolic hydrochloride into the weak cation exchange column. (yield 40%)

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in 1,2-propanediol (1.2 L) is heated to reflux. A Dean-Stark trap is used to withdraw the first 120 mL of condensed solvent. The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which maybe determined by 1H NMR). The solution is cooled and is concentrated under vacuum. Ethanol is used to completely dissolve the α-amino-ε-caprolactam 2. Byproduct NaCl is removed by filtration. The filtrate is concentrated and the resulting crude α-amino-ε-caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (36.5 g) in 74% yield. is heated to reflux to withdraw the first 120 mL of condensed solvent The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which The solution is cooled is concentrated under vacuum to completely dissolve the α-amino-ε-caprolactam 2 Byproduct NaCl is removed by filtration The filtrate is concentrated the resulting crude α-amino-ε-caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in hexanol (1.2 L) is heated to reflux with a Dean-Stark trap used to remove H2O. The suspension is refluxed for 8 hours until all starting material is consumed (which maybe determined by 1H NMR). The suspension is then cooled and filtered to remove byproduct NaCl. The filtrate is concentrated and the resulting crude α-amino-ε-caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (37 g) in 75% yield. is heated to reflux with a Dean-Stark trap to remove H2O The suspension is refluxed for 8 hours until all starting material is consumed (which The suspension is then cooled filtered to remove byproduct NaCl The filtrate is concentrated the resulting crude α-amino-ε-caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in 1,2-propanediol (1.2 L) is heated to reflux. A Dean-Stark trap is used to withdraw the first 120 mL of condensed solvent. The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which maybe determined by 1 H NMR). The solution is cooled and is concentrated under vacuum. Ethanol is used to completely dissolve the α-amino-ε-caprolactam 2. Byproduct NaCl is removed by filtrat is concentrated and the resulting crude α-amino-εcaprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (36.5 g) in 74% yield. is heated to reflux to withdraw the first 120 mL of condensed solvent The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which The solution is cooled is concentrated under vacuum to completely dissolve the α-amino-ε-caprolactam 2 Byproduct NaCl is removed by filtrat is concentrated the resulting crude α-amino-εcaprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in 1,2-propanediol (1.2 L) is heated to reflux. A Dean-Stark trap is used to withdraw the first 120 mL of condensed solvent. The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which maybe determined by 1 H NMR). The solution is cooled and is concentrated under vacuum. Ethanol is used to completely dissolve the α-amino-ε-caprolactam 2. Byproduct NaCl is removed by filtrat is concentrated and the resulting crude α-amino-εcaprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (36.5 g) in 74% yield. is heated to reflux to withdraw the first 120 mL of condensed solvent The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which The solution is cooled is concentrated under vacuum to completely dissolve the α-amino-ε-caprolactam 2 Byproduct NaCl is removed by filtrat is concentrated the resulting crude α-amino-εcaprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in hexanol (1.2 L) is heated to reflux with a Dean-Stark trap used to remove H2O. The suspension is refluxed for 8 hours until all starting material is consumed (which maybe determined by 1 H NMR). The suspension is then cooled and filtered to remove byproduct NaCl. The filtrate is concentrated and the resulting crude α-amino-ε-caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature to afford α-amino-εcaprolactam hydrochloride (37 g) in 75% yield. is heated to reflux with a Dean-Stark trap to remove H2O The suspension is refluxed for 8 hours until all starting material is consumed (which The suspension is then cooled filtered to remove byproduct NaCl The filtrate is concentrated the resulting crude α-amino-ε-caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in 1,2-propanediol (1.2 L) is heated to reflux. A Dean-Stark trap is used to withdraw the first 120 mL of condensed solvent. The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which maybe determined by 1H NMR). The solution is cooled and is concentrated under vacuum. Ethanol is used to completely dissolve the α-amino-ε-caprolactam 2. Byproduct NaCl is removed by filtration. The filtrate is concentrated and the resulting crude α-amino-ε caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (36.5 g) in 74% yield. is heated to reflux to withdraw the first 120 mL of condensed solvent The reaction solution is refluxed for an additional 2 hours until all starting material is consumed (which The solution is cooled is concentrated under vacuum to completely dissolve the α-amino-ε-caprolactam 2 Byproduct NaCl is removed by filtration The filtrate is concentrated the resulting crude α-amino-ε caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and subsequent partial concentration, crystals maybe formed at room temperature

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

实验步骤: A stirred mixture of L-lysine hydrochloride 1 (55 g, 300 mmol) and NaOH (12 g, 300 mmol) in hexanol (1.2 L) is heated to reflux with a Dean-Stark trap used to remove H2O. The suspension is refluxed for 8 hours until all starting material is consumed (which maybe determined by 1H NMR). The suspension is then cooled and filtered to remove byproduct NaCl. The filtrate is concentrated and the resulting crude α-amino-ε-caprolactam 2 is dissolved in water. After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature to afford α-amino-ε-caprolactam hydrochloride (37 g) in 75% yield. is heated to reflux with a Dean-Stark trap to remove H2O The suspension is refluxed for 8 hours until all starting material is consumed (which The suspension is then cooled filtered to remove byproduct NaCl The filtrate is concentrated the resulting crude α-amino-ε-caprolactam 2 is dissolved in water After acidification to pH 6 with addition of concentrated HCl and partial concentration, crystals maybe formed at room temperature

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

实验步骤: The contents, taken out from the glass ampule, were neutralized to about pH 8.0 by adding sodium ethylate-ethanol solution, and the mixture of α-amino-ε-caprolactam hydrochloride, lysine ethyl ester monohydrochloride, and a small amount of lysine ethyl ester dihydrochloride, was obtained. α-amino-ε-caprolactam hydrochloride, lysine ethyl ester dihydrochloride, and sodium chloride were eluted by passing the mixture through the weak cation exchange column, Amberlite IRC-50, freed from water before use, and washing the column with ethanol. Then, 1.18 grs. of lysine ethyl ester monohydrochloride was eluted in the form of the dihydrochloride salt by charging ethanolic hydrochloride into the weak cation exchange column. (yield 40%)