HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2096747Generated: October 31, 2026
Ethyl 4-piperidinecarboxylate → HCID 66697232, compound
https://huagongshe.com/reaction/2096747
Participants
| Role | Name | HCID | Charge |
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| Reactant | Ethyl 4-piperidinecarboxylate | HCID 70770 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 6-[2-(4-Bromo-2-chloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-4-methyl-4H-benzo[1,4]oxazin-3-one | HCID 66697186 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66697232 | HCID 66697232 | 3.2% |
Reaction Steps
To a suspension of 2,2′-bis(diphenylphosphino)-1,1′binaphthyl (3.1 mg), tris(dibenzylideneacetone)dipalladium (0) (1.5 mg) and sodium-tert.-butylate (19 mg) in toluene (15 ml) were added 6-[2-(4-bromo-2-chloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-4-methyl-4H-benzo[1,4]oxazin-3-one (Example 22, step 3, 80 mg) and ethyl piperidine-4-carboxylate (29 mg). The mixture was stirred at room temperature overnight. 2,2′-Bis(diphenylphosphino)-1,1′binaphthyl (3.1 mg), ethyl piperidine-4-carboxylate (29 mg) and tris(dibenzylideneacetone)dipalladium (0) (1.5 mg) were added and the mixture was stirred at 80° C. for 4 h. After cooling to room temperature, the mixture was diluted with EtOAc. The organic phase was washed with water, dried (MgSO4), filtered and concentrated to dryness. The product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>4:1) to give the title compound (3 mg) as light yellow oil. MS (m/e)=555.3 [M+H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08450313B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-d8e4b7762e3d4ca098cbe25f8a51b1f6 |
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| Source note | uspto-grants-2013_05 |
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