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CAS No. : | 771-99-3 | MDL No. : | MFCD00006002 |
Formula : | C11H15N | Boiling Point : | No data available |
Linear Structure Formula : | C6H5CH(CH2)4NH | InChI Key : | UTBULQCHEUWJNV-UHFFFAOYSA-N |
M.W : | 161.24 | Pubchem ID : | 69873 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium bicarbonate; sodium chloride; triethylamine; In tetrahydrofuran; ethanol; | 3) Synthesis of 1-[4-[N-(tert-butoxycarbonyl)aminomethyl]benzyl]-4-phenylpiperidine To a solution of 5.0 g (21.07 mM) of <strong>[123986-64-1]4-[N-(tert-butoxycarbonyl)aminomethyl]-1-phenylmethanol</strong> and 5.9 ml (42.33 mM) of triethylamine in THF (42 ml) was added 2.5 ml (32.3 mM) of methanesulfonyl chloride at 0° C. and the mixture was stirred at the prevailing temperature for one hour. The reaction was then stopped by adding saturated aqueous solution of sodium hydrogen carbonate and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over MgSO4. The solvent was then distilled off under reduced pressure to provide 6.72 g (21.07 mM) of crude product as light-brown solid. To a solution of 6.72 g (21.07 mM) of this crude mesylate in ethanol (42 ml) was added 5.9 ml (42.33 mM) of triethylamine as well as 3.40 g (21.09 mM) of 4-phenylpiperidine and the mixture was refluxed for 18 hours. After cooling to room temperature, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After concentration, the crude product was purified by column chromatography (ethyl acetate-hexane: 50percent) to provide the title compound as light-yellow solid. Yield 5.77 g (72percent) m.p. 73-74° C. 1H-NMR (200 MHz, CDCl3) delta: 1.46 (9H, s), 1.73-1.88 (4H, m), 1.99-2.19 (1H, m), 2.94-3.08 (2H, m), 3.54 (2H, s), 4.31 (2H, d, J=5.8 Hz), 4.73-4.96 (1H, m), 7.13-7.36 (4H, m). IR (KBr): 3389, 1690, 1518, 1269, 1171 cm-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium bicarbonate; sodium chloride; triethylamine; In tetrahydrofuran; ethanol; | 1) Synthesis of 1-[4-[N-(tert-butoxycarbonyl)aminomethyl]benzyl]-4-benzylpiperidine To a solution of 5.0 g (21.07 mM) of <strong>[123986-64-1]4-[N-(tert-butoxycarbonyl)aminomethyl]-1-phenylmethanol</strong> and 5.9 ml (42.33 mM) of triethylamine in THF (42 ml) was added 2.5 ml (32.3 mM) of methanesulfonyl chloride at 0° C. and the mixture was stirred at the prevailing temperature for one hour. The reaction was stopped by adding saturated aqueous solution of sodium hydrogen carbonate and the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over MgSO4. The solvent was then distilled off under reduced pressure to provide 7.21 g (21.07 mM) of crude product as light-brown solid. To a solution of 7.21 g (21.07 mM) of this crude mesylate in ethanol (42 ml) was added 5.9 g (42.33 mM) of triethylamine as well as 3.69 g (21.05 mM) of 4-phenylpiperidine and the mixture was refluxed for 18 hours. After cooling to room temperature, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over MgSO4. After concentration, the crude product was purified by column chromatography (ethyl acetate-hexane: 50percent) to provide the title compound as light-yellow oil. Yield 5.77 g (69percent) 1H-NMR (200 MHz, CDCl3) delta: 1.20-1.40 (2H, m), 1.46 (9H, s), 1.85-2.01 (2H, m), 2.53 (2H, d, J=6.2 Hz), 2.78-2.93 (2H, m), 3.48 (2H, s), 4.29 (2H, d, J=6.0 Hz), 4.70-4.88 (1H, m), 7.07-7.34 (9H, m). IR (neat): 3350, 2924, 1709, 1508, 1452, 1365, 1252, 1173 cm-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
53% | To a solution of NaH (0.193 g, 4.834 mmol) in DMF (20 ml) cooled at 0 0C, was added 4-phenylpiperidine (0.844 g, 5.236 mmol) was added. The resulting reaction mixture was stirred at 0 0C for 10 min., before D25 (0.87 g, 4.028 mmol) was added. The resulting mixture was warmed to r.t. and stirred for 1 h.. The mixture was then quenched with water and extracted with Et2O. The organic layer was separated, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 2% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D33 (0.73 g, 53%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
2-(4-phenylpiperidin-1-yl)-4-trifluoromethyloxazole-5-carboxylic Acid (A-22) Intermediate A-22 was prepared by the general procedure for intermediate A-4, by using A-2 and 4-phenylpiperidine as starting materials. MS (M+1): 341. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A solution of 3-(4-Phenyl-2,5-dioxo-imidazolidin-4-yl)propionic acid (30mg, 0.12 mmol, 1 eq.), TEA (51 jiL, 0.35 mmol, 3eq.) and HOBT (18mg, 0.13 mmol, 1.1 eq) in DMF is stirred at room temperature for 5 mm. EDC-HC1 (28mg, 0.1 Smmol, 1.2 eq) is then added and the mixture is stirred at room temperature for 15 mm. 4-phenylpiperidine in solution in minimum amount of DMF is then added, and the reaction mixture is stirred at room temperature overnight. Solvent are evaporated under reduced pressure, and crude compound is then purified by LC/MS preparative purification, to afford expected Cpd 3. LCMS: MW (calcd): 391; m/z MW (obsd): 392 (M+H). |
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