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CAS No. : | 28566-14-5 | MDL No. : | MFCD07371500 |
Formula : | C8H7NO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | LMEREVKJVWUGJI-UHFFFAOYSA-N |
M.W : | 133.15 | Pubchem ID : | 1512521 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H317-H319 | 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 |
---|---|---|
1.14 g | To a 0 C solution of 6,7-dihydro-5H-cyclopenta[b]pyridin-5-one (1.70 g, 12.77 mmol) in DMF (20 mL) under nitrogen atmosphere was added NaH (60% dispersion in mineral oil, 982 mg, 24.55 mmol) in three portions, and the mixture was heated to 60 C, stirred for 1 h at thistemperature. Then <strong>[24468-88-0]N-benzyl-2-bromo-N-(2-bromoethyl)ethan-1-amine</strong> (4.54 g, 14.14 mmol) was added and stirred at 60 C for another 1 h. After cooling to RT, the reaction mixture was quenchedwith water (80 mL), extracted with EA (3 > 80 mL). The combined organic layers were washed with water (3 x 80 mL), dried over anhydrous Na2504, filtered and concentrated under reduced pressure. The residue was purified by silica chromatography (eluting with EA) to give1?-benzylspiro[cyclopenta[b]pyridine-6,4?-piperidin]-5(7H)-one (1.14 g). MS: m/z 293 (M+H). | |
1.14 g | 6,7-Dihydro-5H-cyclopenta[b]pyridin-5-one (1.70 g, 12.77 mmol) in DMF (20 mL) at 0 CSodium hydride (60% mineral oil dispersion, 982 mg, 24.55 mmol) was added to the solution in three portions, then the mixture was heated to 60 C and stirred at this temperature for 1 h.N-Benzyl-2-bromo-N-(2-bromoethyl)ethane-1-amine (4.54 g, 14.14 mmol) was then added and stirred at 60 C for further 1 h.After cooling to RT, the reaction was quenched with water (80 mL).Extract with EA (3 x 80 mL). The combined organic phases were washed with water (3×80 mL).Dry over anhydrous Na2SO4, filtered and evaporated.The residue was purified by silica gel chromatography eluting with EtOAc.1'-Benzylspiro[cyclopenta[b]pyridine-6,4'-piperidine]-5(7H)-one (1.14 g) was obtained. |
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