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CAS No. : | 5382-17-2 | MDL No. : | MFCD00035298 |
Formula : | C5H12ClNO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | VKCORPXOKYDINR-UHFFFAOYSA-N |
M.W : | 137.61 | Pubchem ID : | 16212499 |
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: |
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* 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 benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; N-ethyl-N,N-diisopropylamine; In DMF (N,N-dimethyl-formamide); at 20℃; for 16.0h; | To a stirred solution OF BOC-3- (4-FLUOROPHENYL)- (S)-ALANINE (LO. OG, 35. 3MMOL), <strong>[5382-17-2]4-hydroxypiperidine hydrochloride</strong> (5. 1G, 37. 1MMOL) and HOBt (7.2g, 52. 9MMOL) in DMF (lOOmL), was added DIPEA (12. 3mL, 70. 6MMOL) and after 5MIN, EDCI (7.4g, 38. 8MMOL) and the reaction stirred at rt for 16H. The solvent was removed in vacuo and the residue partitioned between water (150ML) and ethyl acetate (2 x 150ML). The combined organic fractions were washed with sodium hydroxide solution (2M, 50ML), hydrochloric acid (2N, 50ML), dried (MGS04) and concentrated in vacuo. The product was chromatographed on silica gel eluting with ethyl acetate to give the title compound as a white solid. m/z (ES+) = 367 [M+ H] + ; RT = 3.28min. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium carbonate; In dichloromethane; water; at 0℃; for 1.08333h; | Preparation 11: 4-Hydroxypiperidine-l-carbonitrileA stirred slurry OfNa2CO3 (9.8 g, 117 mmol) in water (15 mL) was cooled on ice-water and 4-hydroxypiperidine.HCl (4.0 g, 29.2 mmol) was added. A solution of cyanogen bromide(3.7 g, 35 mmol) in CH2Cl2 (90 mL) was added portionwise over 5 min and the stirring continued for 1 h. The reaction was diluted with CH2Cl2 ( 100 mL), the organic phase separated and dried (MgSO-O and the solvent evaporated to afford the title cyanamide: SH (CDCl3) 1.65 (ddt, 2H), 1.91 (ddt, 2H), 2.17 (br s, IH), 3.08 (ddd, 2H), 3.45 (ddd, 2H), 3.86 (sept, IH). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With N-ethyl-N,N-diisopropylamine; In acetonitrile; at 60℃; for 18.0h; | A solution of 4-(3-bromo-propyl)-phenol (EXAMPLE 6; 1.42 g, 6.6 mmol), <strong>[5382-17-2]4-hydroxypiperidine hydrochloride</strong> (908 mg, 6.6 mmol), and N,N-diisopropylethyamine (2.2 mL, 12.3 mmol) in CH3CN (20 mL) was stirred at 60° C. for 18 h. The reaction mixture was cooled to room temperature, and the solvent was removed under reduced pressure to yield an off-white solid. This material was dissolved in CH2Cl2 (200 mL), and the solution was washed with H2O (2.x.50 mL), dried (Na2SO4), filtered and concentrated under reduce pressure to yield a white solid. Diethyl ether was added, and the title compound was collected by filtration (1.4 g, 90percent yield). TLC (SiO2, 5percent 2 M NH3 in CH3OH/CH2Cl2): Rf=0.05. MS (ESI): mass calculated for C14H21NO2, 235.16; m/z found, 236.2 [M+H]+. 1H NMR (400 MHz, CD3OD): 6.96-6.94 (m, 2H), 6.64-6.61 (m, 2H), 3.89-3.82 (m, 1H), 3.29-3.20 (m, 4H), 3.02-2.95 (m, 4H), 2.52 (t, J=7.4, 2H), 1.95-1.87 (m, 4H), 1.68-1.60 (m, 2H). |
90% | With N-ethyl-N,N-diisopropylamine; In acetonitrile; at 60℃; for 18.0h; | EXAMPLE 36; 1- {3- [4- (BENZOOXAZOL-2-YLOXY)-PHENYL]-PROPYL}-PIPERIDIN-4-OL; A. 1-F3- 4-HVDROXV-PHENYL)-PROPY]-PIPERIDIN-4-OL; A SOLUTION of 4- (3-bromo- propyl)-phenol (EXAMPLE 6; 1.42 g, 6.6 MMOL), <strong>[5382-17-2]4-hydroxypiperidine hydrochloride</strong> (908 mg, 6.6 mmol), and N, N-diisopropylethyamine (2.2 mL, 12.3 MMOL) in CH3CN (20 mL) was stirred at 60 °C for 18 h. The reaction mixture was cooled to room temperature, and the solvent was removed under reduced pressure to yield an off-white solid. This material was dissolved in CH2CI2 (200 mL), and the solution was washed with H20 (2 x 50 mL), dried (Na2SO4), filtered and concentrated under reduce pressure to yield a white solid. Diethyl ether was added, and the title compound was collected by filtration (1.4 g, 90percent yield). TLC(SiO2, 5percent 2 M NH3 in CH3OH/CH2Cl2) : Rf = 0. 05. MS (ESI) : mass calculated for C14H21NO2, 235.16 ; m/z found, 236.2 [M+H] +. H NMR (400 MHz, CD30D) : 6.96-6. 94 (m, 2H), 6.64-6. 61 (m, 2H), 3.89-3. 82 (m, 1 H), 3.29- 3.20 (m, 4H), 3.02-2. 95 (m, 4H), 2.52 (t, J = 7.4, 2H), 1.95-1. 87 {M, 4H), 1.68- 1.60 (m, 2H) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hydrogencarbonate; In ethanol; water; at 80℃; for 5.0h; | 150 mg of the above chloroethylaminoamide, 400 mg of <strong>[5382-17-2]4-hydroxypiperidine hydrochloride</strong> and 800 mg of sodium bicarbonate in 5 mL of ethanol/water (95/5) was stirred at: 80° C. for 5 h, filtered and evaporated. The residue was purified on preparative TLC (10percent[aq.NH4OH/MeOH 1/9]/DCM), 72 mg of the desired product was obtained as an gummy solid. It was converted into hydrochloride salt with 4N HCl/dioxane and delivered for bioassays. Mass Spectrum (NH3-CI): m/z 466.2 (M+1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 4-methyl-morpholine; 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride; In ethanol; at 20℃; for 16.0h; | Example 28: 5-Chloro-lH-pyrrolo[2,3-c]pyridine-2-carboxylic acid {l-[2-(4-hydroxypiperidin- l-yl)-2-oxoethyl]-2-oxo-l,2,3,4-tetrahydroquinolin-3-yl}amide; DMTMM (83mg, 0.30mmol) was added to a stirred solution of {3-[(5-chloro-lH-pyrrolo[2,3- c]pyridine-2-carbonyl)amino]-2-oxo-3,4-dihydro-2H-quinolin-l-yl}acetic acid (Example 22, lOOmg, 0.25mmol) and <strong>[5382-17-2]4-hydroxypiperidine hydrochloride</strong> (38mg, 0.28mmol) in ethanol (1OmL) and 4- methylmorpholine (30muL, 0.28mmol). The reaction was stirred at rt for 16h. The solvent was removed in vacuo and the residue triturated with H2O affording the title compound as a white solid, m/z (ES+) 482 [M+H]+; RT = 2.97min. |
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