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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of (2S,4R)-4-fluoropyuolidine~2~carboxylic acid (0.50 g} 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (CELITE) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap- 11 as a white solid (337.7 mg). 1H NMR (DMSOd6, delta = 2.5, 500 MHz) 5.39 (d m, J=53.7, IH), 4.30 (m, IH), 3.90 (ddd, /=31.5, 13.5, 4.5, IH), 3.33 (dd, J=25.6, 13.4, IH), 2.85 (s, 3H), 2.60-2.51 (m, IH), 2.39-2.26 (m, IH). RT=0.28 (Cond. II); >;98% homogeneity index; LC/MS: Anal. Calcd. for [M+H)+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O)5 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (CELITE) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap-1 1 as a white solid (337.7 mg). 'H NMR (DMSO-d6, 5=2.5, 500 MHz) 5.39 (d m, J=53.75 IH), 4.30 (m, IH), 3.90 (ddd, j=31.5, 13.5, 4.5, 1H)} 3.33 (dd, J=25.6, 13.4, IH), 2.85 (s, 3H), 2.60-2.51 (m, IH), 2.39-2.26 (m, IH). RT-0.28 (Cond. II); >;98% homogeneity index; LC/MS: Anal Calcd. for [M+H]+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H20), 12 N HC1 (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (CELITE) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HC1 salt of Cap- 1 1 as a white solid (337.7 mg). 1H NMR (DMSO-d6, 5=2.5, 500 MHz) 5.39 (d m, J=53.7, 1H), 4.30 (m, 1H), 3.90 (ddd, J=31.5, 13.5, 4.5, 1H), 3.33 (dd, J=25.6, 13.4, 1H), 2.85 (s, 3H), 2.60-2.51 (m, 1H), 2.39-2.26 (m, 1H). RT=0.28 (Cond. II); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6HnFN02: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H20), 12 N HC1 (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (CELITE) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HC1 salt of Cap-1 1 as a white solid (337.7 mg). 1H NMR (DMSO-d6, delta=2.5, 500 MHz) 5.39 (d m, J=53.7, 1H), 4.30 (m, 1H), 3.90 (ddd, J=31.5, 13.5, 4.5, 1H), 3.33 (dd, J=25.6, 13.4, 1H), 2.85 (s, 3H), 2.60-2.51 (m, 1H), 2.39-2.26 (m, 1H). RT=0.28(Condition II); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6H11FN02: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H20), 12 N HC1 (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HC1 salt of Cap-1 1 as a white solid (337.7 mg). XH NMR (DMSO-d6, 5=2.5, 500 MHz) 5.39 (d m, J=53.7, 1H), 4.30 (m, 1H), 3.90 (ddd,J=31.5, 13.5, 4.5, 1H), 3.33 (dd, J=25.6, 13.4, 1H), 2.85 (s, 3H), 2.60-2.51 (m, 1H), 2.39-2.26 (m, 1H). RT=0.28 (Cond. II); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6HnFN02: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap-11 as a white solid (337.7 mg). 1H NMR (DMSO-d6, delta=2.5, 500 MHz) 5.39 (d m, J=53.7, 1H), 4.30 (m, 1H), 3.90 (ddd, J=31.5, 13.5, 4.5, 1H), 3.33 (dd, J=25.6, 13.4, 1H), 2.85 (s, 3H), 2.60-2.51 (m, 1H), 2.39-2.26 (m, 1H). RT=0.28 (Cond. 2); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite R) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap-11 as a white solid (337.7 mg). 1H NMR (DMSO-d6, delta=2.5, 500 MHz) 5.39 (d m, J=53.7, IH), 4.30 (m, IH), 3.90 (ddd, .7=31.5, 13.5, 4.5, IH), 3.33 (dd, J=25.6, 13.4, IH), 2.85 (s, 3H), 2.60-2.51 (m, IH), 2.39-2.26 (m, IH). RT=0.28 (Cond. II); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
Cap-11A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite ) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap-l 1 as a white solid (337.7 mg). 1H NMR (DMSO-d6, delta = 2.5, 500 MHz) 5.39 (d m, J = 53.7, IH), 4.30 (m, IH), 3.90 (ddd, J = 31.5, 13.5, 4.5, IH), 3.33 (dd, J = 25.6, 13.4, IH), 2.85 (s, 3H), 2.60-2.51 (m, IH), 2.39-2.26 (m, IH). RT = 0.28 (Com. 2); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap-11 as a white solid (337.7 mg). 1H NMR (DMSO-d6, delta=2.5, 500 MHz) 5.39 (d m, J=53.7, 1H), 4.30 (m, 1H), 3.90 (ddd, J=31.5, 13.5, 4.5, 1H), 3.33 (dd, J=25.6, 13.4, 1H), 2.85 (s, 3H), 2.60-2.51 (m, 1H), 2.39-2.26 (m, 1H). RT=0.28 (Cond. II); >98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6H11FNO2: 148.08; found 148.06. |
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With hydrogenchloride; hydrogen;palladium 10% on activated carbon; In methanol; water; for 19h; |
A mixture of <strong>[2438-57-5](2S,4R)-4-fluoropyrrolidine-2-carboxylic acid</strong> (0.50 g, 3.8 mmol), formaldehyde (0.5 mL of 37% wt. in H2O), 12 N HCl (0.25 mL) and 10% Pd/C (50 mg) in methanol (20 mL) was stirred under a balloon of hydrogen for 19 hours. The reaction mixture was filtered through diatomaceous earth (Celite) and the filtrate was concentrated in vacuo. The residue was recrystallized from isopropanol to provide the HCl salt of Cap- 11 as a white solid (337.7 mg). 1H NMR (DMSO-dbeta, delta=2.5, 500 MHz) 5.39 (d m, 7=53.7, IH), 4.30 (m, IH), 3.90 (ddd, J=31.5, 13.5, 4.5, IH)5 3.33 (dd, J-25.6, 13.4, IH), 2.85 (s, 3H), 2.60-2.51 (m, IH), 2.39-2.26 (m, IH). RT-0.28 (Cond. II); >;98% homogeneity index; LC/MS: Anal. Calcd. for [M+H]+ C6HnFNO2: 148.08; found 148.06. |