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With palladium (II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-I -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9Muorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgSθ4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a BIOTAGE purification (350 g silica gel, CH2Cl2 elution) to afford (S)-l-benzyl 4- methyl 2-(9-phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSOd6, δ - 2.5 ppm, 400 MHz); δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, IH), 4.51 (d, J = 12.6, IH), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, IH), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C31H28NO4: 478.20; found 478.19. |
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With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
Cap-80.a; Cap-80.b
Pb(N03)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2C12 (80 mL) solution of (S)-l -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgS04 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to aBIOTAGE purification (350 g silica gel, CH2C12 elution) to afford (S)-l -benzyl 4- methyl 2-(9-phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 'H NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, 1H), 4.51 (d, J = 12.6, 1H), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C3iH28N04: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
80a/b
Pb(N03)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2C12 (80 mL) solution of (S)-l -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3 (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgS04 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a BIOTAGE purification (350 g silica gel, CH2C12 elution) to afford (S)-l -benzyl 4-methyl 2-(9- phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, 1H), 4.51 (d, J = 12.6, 1H), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50- 2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C31H28N04: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
[00204] Pb(N03)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2C12 (80 mL) solution of (S)-l -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3 (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgS04 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a BIOTAGE purification (350 g silica gel, CH2C12 elution) to afford (S)-l -benzyl 4-methyl 2-(9- phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). ¾ NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, 1H), 4.51 (d, J = 12.6, 1H), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50- 2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC-MS: Anal. Calcd. for [M+H]+ C3iH28N04: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
Pb(N03)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2C12 (80 mL) solution of (S)-l -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and EtsN (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgS04 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a Biotage purification (350 g silica gel, CH2C12 elution) to afford (S)-l -benzyl 4-methyl 2-(9- phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). XH NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, 1H), 4.51 (d, J = 12.6, 1H), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C3iH28N04: 478.20; found 478.19. |
| 7.93 g |
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
80a; 80b
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-1-benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9-phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol),and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate wastreated with MgSO4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submittedto a Biotage purification (350 g silica gel, CH2Cl2 elution) to afford (S)-1-benzyl 4-methyl 2-(9-phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H),7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, 1H), 4.51 (d, J = 12.6, 1H), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H),2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+C31H28NO4: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-1-benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9-phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgSO4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a Biotage purification (350 g silica gel, CH2Cl2 elution) to afford (S)-1-benzyl 4-methyl 2-(9-phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ=2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J=12.4, 1H), 4.51 (d, J=12.6, 1H), 3.78 (d, J=9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT=2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C31H28NO4: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48h; |
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-I -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgSO4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a Biotage purification (350 g silica gel, CH2CI2 elution) to afford (S)-I -benzyl 4-methyl 2-(9- phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, IH), 4.51 (d, J = 12.6, IH), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, IH), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C3IH28NO4: 478.20; found 478.19. |
|
With lead nitrate; triethylamine In dichloromethane at 20℃; for 48.0167h; |
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-I -benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9- phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgSO4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a Biotage purification (350 g silica gel, Cη2CI2 elution) to afford (S)-I -benzyl 4-methyl 2-(9- phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ = 2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J = 12.4, IH), 4.51 (d, J = 12.6, IH), 3.78 (d, J = 9.1, NH), 3.50 (s, 3H), 2.99 (m, IH), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT = 2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C3IH28NO4: 478.20; found 478.19. |
|
With lead(II) nitrate; triethylamine In dichloromethane at 20℃; for 48.0167h; |
80a; 80b
Pb(NO3)2 (6.06 g, 18.3 mmol) was added over 1 min to a CH2Cl2 (80 mL) solution of (S)-1-benzyl 4-methyl 2-aminosuccinate (4.50 g, 19.0 mmol), 9-bromo-9-phenyl-9H-fluorene (6.44 g, 20.0 mmol) and Et3N (3.0 mL, 21.5 mmol), and the heterogeneous mixture was stirred at ambient condition for 48 hr. The mixture was filtered and the filtrate was treated with MgSO4 and filtered again, and the final filtrate was concentrated. The resulting crude material was submitted to a Biotage purification (350 g silica gel, CH2Cl2 elution) to afford (S)-1-benzyl 4-methyl 2-(9-phenyl-9H-fluoren-9-ylamino)succinate as highly viscous colorless oil (7.93 g). 1H NMR (DMSO-d6, δ=2.5 ppm, 400 MHz): δ 7.82 (m, 2H), 7.39-7.13 (m, 16H), 4.71 (d, J=12.4, 1H), 4.51 (d, J=12.6, 1H), 3.78 (d, J=9.1, NH), 3.50 (s, 3H), 2.99 (m, 1H), 2.50-2.41 (m, 2H, partially overlapped with solvent). LC (Cond. 1): RT=2.16 min; LC/MS: Anal. Calcd. for [M+H]+ C31H28NO4: 478.20; found 478.19. |
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