HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl 3,3-dimethyl-4-oxopiperidine-1-carboxylate → 4-(4-Chloro-phenyl)-4-hydroxy-3,3-dimethyl-piperidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl 3,3-dimethyl-4-oxopiperidine-1-carboxylate | HCID 22278899 | — |
| Reactant | HCID 178478191 | HCID 178478191 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(4-Chloro-phenyl)-4-hydroxy-3,3-dimethyl-piperidine-1-carboxylic acid tert-butyl ester | HCID 59341212 | — |
Reaction Steps
To an ice-cooled solution 3,3-Dimethyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester (1.6 g, 7.2 mmol) in THF (20 mL) was added 4-chlorophenylmagnesium bromide (1 M in ether, 15 mL, 15 mmol). The solution was allowed to warm to about room temperature, then stirred at room temperature for about 22 hours. The reaction was quenched with aqueous ammonium chloride and extracted with ethyl acetate. The combined organic layers were concentrated in vacuo, then purified by flash chromatography on silica gel (35 g SiO2, gradient elution from 100% hexane to 100% ethyl acetate) to yield the title compound as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653096B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-78bdd389d3534e50b6c0cd096fb8ef8e |
| Source note | uspto-grants-2014_02 |