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CAS No. : | 59184-90-6 | MDL No. : | MFCD02183575 |
Formula : | C9H17NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IHSUFLCKRIHFGY-UHFFFAOYSA-N |
M.W : | 171.24 | Pubchem ID : | 2760465 |
Synonyms : |
|
Chemical Name : | Ethyl 2-(piperidin-4-yl)acetate |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
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 caesium carbonate; In N,N-dimethyl-formamide; at 20 - 55℃;Inert atmosphere; | Step A: ethyl \\ 1 -(5 -chloropyrazm-2-y )piperidm-4-yl] acetate2,5-Dichloropyrazine (1.42 g, 9.53 mmol, 1.0 equiv.) and ethyl piperidin-4-ylacetate(1.66 g, 9.69 mmol, 1.02 equiv.) were dissolved in DMF (23 mL) and stirred at roomtemperature. Cesium carbonate (5.0 g, 15.35 mmol, 1.61 equiv.) was added and the resulting reaction suspension was stirred in a 55°C oil bath for 3 hrs while under N2(g)- The reaction suspension was filtered to remove solids and to collect the DMF solution, which was mostly concentrated to a suspension. The suspension was dissolved in EtOAc / 13/40. After shaking, theEtOAc phase was dried over Na2S04, filtered, and concentrated to a residue. Purification with Biotage SP-1 [ SNAP lOOg cartridge Hexanes:EtOAc 0 > 10percent 2CV; 10 > 80percent 10CV; 80percent 2CV ] isolated the desired product. LC-MS (ES, m z): Ci3Hl8ClN302: 283; Found: 284[M+Hf. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In tetrahydrofuran; at 20℃; | General procedure: To a solution of <strong>[10241-97-1]5-methyl-1H-indole-2-carboxylic acid</strong> (20) (263mg, 1.50mmol) in THF (7mL) were added 2-(piperidin-4-yl)ethanol (213mg, 1.65mmol), 1-hydroxybenzotriazole (HOBt, 101mg, 0.750mmol), and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDAC) hydrochloride (316mg, 1.65mmol), followed by stirring at room temperature for 14h. The reaction mixture was partitioned between ethyl acetate and 0.5M aqueous hydrochloric acid. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then concentrated in vacuo. The residue was recrystallized from ethyl acetate/acetonitrile (5mL/2mL) to give 3 (365mg, 85.0percent) as a beige powder. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
3.98 g | With sodium hydrogencarbonate; In 1-methyl-pyrrolidin-2-one; at 20℃; | Step 1. Ethyl [ 1 -(5 -nitropyridin-2-yl)piperidin-4-yl] acetate To a solution of <strong>[456-24-6]2-fluoro-5-nitropyridine</strong> (2.000 g, 14.08 mmol) and 2-(piperidine-4-yl)-acetic acid ethyl ester (2.410 g, 14.08 mmol) in 30 mL NMP was added sodium bicarbonate (3.5 g, 42.2 mmol). The reaction mixture was stirred at RT over night and was worked up using EtOAc extraction following addition of water. The crude product thus obtained was purified on silica gel using 0-50percent gradient of EtOAc to give 3.98 g title compound as a bright yellow solid. LC-MS: 1.75 min. (LC4, m/Z 294.15). 1H NMR (CDC13, 500 MHz) delta 9.02 (d, 2.8 Hz, IH), 8.18 (dd, 9.5 & 2.8 Hz, IH), 6.56 (d, 9.6 Hz, IH), 4.53 (br d, 12.0 Hz, 2H), 4.15 (q, 7.1 Hz, 2H), 3.01-3.06 (m, 2H), 2.28 (d, 7.1 Hz, 2H), 2.1 1-2.21 (m, IH), 1.89 (d, 13.0 Hz, 2H), 1.27 (t, 7.1 Hz, 3H), 1.24-1.33 (m, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; for 0.5h;Microwave irradiation; Inert atmosphere; | The compound ethyl 2-(piperidin-4-yl)acetate (500 mg, 2.92 mmol),<strong>[661463-17-8]4-bromo-6-fluoroquinoline</strong> (791.2 mg, 3.5 mmol),Tris(dibenzylideneacetone)dipalladium (267.5 mg, 0.292 mmol),4,5-bisdiphenylphosphino-9,9-dimethyloxaxan (338 mg, 0.584 mmol),Cesium carbonate (1.89 g, 5.89 mmol) and 1,4-dioxane (10 ml) were mixed and then heated in a microwave reactor for 30 minutes under a nitrogen atmosphere. After the reaction was completed, it was filtered, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether / ethyl acetate = 1/9), To give the desired product 2- (1- (6-fluoro-quinolin-4-yl) piperidin-4-yl) acetate 11b (500mg, yellow solid), yield: 54%. |
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