消旋卡多曲EP杂质F

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

实验步骤: 2.42 g (15 mmoles) of 2-benzyl acrylic acid are dissolved in 30 ml of THF and 10 ml of CHCl3. There is added a solution in 50 ml of THF of 1.87 g of glycine benzyl ester hydrochlorate, 2.2 g of triethylamine, then 2.20 g of HOBT and 3.4 g of DCC. The mixture is stirred for 20 hours at room temperature. The precipitate of DCU formed is collected. After evaporating to dryness and taking up with ethyl acetate the organic phase is washed in succession with 2×20 ml of citric acid, then 3×20 ml of NaHCO3. The material is concentrated under a vacuum and the rest of the DCU formed is suction filtered. A yellow oil which crystallizes slowly is obtained. The precipitate of DCU formed is collected After evaporating to dryness is washed in succession with 2×20 ml of citric acid The material is concentrated under a vacuum the rest of the DCU formed filtered A yellow oil which crystallizes slowly is obtained

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

实验步骤: 2.10 (6.8 mmoles) of N-(2-benzyl propenoyl-glycine benzyl ester, M.P. =60° C, are stirred at 10° C. for 2 hours with a mixture of 30 ml of methanol and 0.27 g of NaOH (6.8 mmoles), dissolved in 5 ml of water. The pH is brought to 1 by the addition of 2N HCl and the material is extracted with ethyl acetate. The solvent is washed with 2×20 ml of water, dried and evaporated under a vacuum. 1.36 g of crystals are obtained. the material is extracted with ethyl acetate The solvent is washed with 2×20 ml of water dried evaporated under a vacuum

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

实验步骤: 2.10 (6.8 mmoles) of N-(2-benzyl propenoyl-glycine benzyl ester, M.P. =60° C, are stirred at 10° C. for 2 hours with a mixture of 30 ml of methanol and 0.27 g of NaOH (6.8 mmoles), dissolved in 5 ml of water. The pH is brought to 1 by the addition of 2N HCl and the material is extracted with ethyl acetate. The solvent is washed with 2×20 ml of water, dried and evaporated under a vacuum. 1.36 g of crystals are obtained. the material is extracted with ethyl acetate The solvent is washed with 2×20 ml of water dried evaporated under a vacuum

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

实验步骤: 2.10 (6.8 mmoles) of N-(2-benzyl propenoyl-glycine benzyl ester, M.P. =60° C, are stirred at 10° C. for 2 hours with a mixture of 30 ml of methanol and 0.27 g of NaOH (6.8 mmoles), dissolved in 5 ml of water. The pH is brought to 1 by the addition of 2N HCl and the material is extracted with ethyl acetate. The solvent is washed with 2×20 ml of water, dried and evaporated under a vacuum. 1.36 g of crystals are obtained. the material is extracted with ethyl acetate The solvent is washed with 2×20 ml of water dried evaporated under a vacuum

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

实验步骤: 2.42 g (15 mmoles) of 2-benzyl acrylic acid are dissolved in 30 ml of THF and 10 ml of CHCl3. There is added a solution in 50 ml of THF of 1.87 g of glycine benzyl ester hydrochlorate, 2.2 g of triethylamine, then 2.20 g of HOBT and 3.4 g of DCC. The mixture is stirred for 20 hours at room temperature. The precipitate of DCU formed is collected. After evaporating to dryness and taking up with ethyl acetate the organic phase is washed in succession with 2×20 ml of citric acid, then 3×20 ml of NaHCO3. The material is concentrated under a vacuum and the rest of the DCU formed is suction filtered. A yellow oil which crystallizes slowly is obtained. The precipitate of DCU formed is collected After evaporating to dryness is washed in succession with 2×20 ml of citric acid The material is concentrated under a vacuum the rest of the DCU formed filtered A yellow oil which crystallizes slowly is obtained

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

实验步骤: 2.42 g (15 mmoles) of 2-benzyl acrylic acid are dissolved in 30 ml of THF and 10 ml of CHCl3. There is added a solution in 50 ml of THF of 1.87 g of glycine benzyl ester hydrochlorate, 2.2 g of triethylamine, then 2.20 g of HOBT and 3.4 g of DCC. The mixture is stirred for 20 hours at room temperature. The precipitate of DCU formed is collected. After evaporating to dryness and taking up with ethyl acetate the organic phase is washed in succession with 2×20 ml of citric acid, then 3×20 ml of NaHCO3. The material is concentrated under a vacuum and the rest of the DCU formed is suction filtered. A yellow oil which crystallizes slowly is obtained. The precipitate of DCU formed is collected After evaporating to dryness is washed in succession with 2×20 ml of citric acid The material is concentrated under a vacuum the rest of the DCU formed filtered A yellow oil which crystallizes slowly is obtained

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

实验步骤: 2.42 g (15 mmoles) of 2-benzyl acrylic acid are dissolved in 30 ml of THF and 10 ml of CHCl3. There is added a solution in 50 ml of THF of 1.87 g of glycine benzyl ester hydrochlorate, 2.2 g of triethylamine, then 2.20 g of HOBT and 3.4 g of DCC. The mixture is stirred for 20 hours at room temperature. The precipitate of DCU formed is collected. After evaporating to dryness and taking up with ethyl acetate the organic phase is washed in succession with 2×20 ml of citric acid, then 3×20 ml of NaHCO3. The material is concentrated under a vacuum and the rest of the DCU formed is suction filtered. A yellow oil which crystallizes slowly is obtained. The precipitate of DCU formed is collected After evaporating to dryness is washed in succession with 2×20 ml of citric acid The material is concentrated under a vacuum the rest of the DCU formed filtered A yellow oil which crystallizes slowly is obtained