HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 905964Generated: October 31, 2026
Dichloromethane → HCID 59363373, compound
https://huagongshe.com/reaction/905964
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Racemic [1-(2,2,2-trifluoro-ethyl)-piperidin-3-yl]-carbamic acid tert-butyl ester | HCID 67386443 | — |
| Product | HCID 59363373 | HCID 59363373 | 94% |
Reaction Steps
To a suspension of the product of step 1 in DCM at 0° C., DIPEA (4 eqv) was added slowly and stirred for 30 minutes at 25° C. The reaction mixture was cooled again to 0° C. and acetyl chloride (1.1 eqv) was added slowly. The resulting mixture was stirred at 25° C. for 16 hrs before being quenched by addition of saturated aqueous NaHCO3. The aqueous layer was back extracted three times with DCM. The combined organics were washed with H2O, dried (Na2SO4), filtered and evaporated. The residue was purified by SiO2 flash chromatography to give racemic 1-acetyl-3-methyl-piperidin-4-one (94% over two steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08012974B2 |
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| Source dataset | uspto-grants-2011_09 |
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| ORD ID | ord-fcecddb673734e6fbecb6ae7b1435cca |
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| Source note | uspto-grants-2011_09 |
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