HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66731635, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Lithium Bromide | HCID 82050 | — |
| Reactant | HCID 66734975 | HCID 66734975 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 66731635 | HCID 66731635 | 91.5% |
Reaction Steps
Dimethyl 2-(2,4-dichlorophenyl)piperidine-1,4-dicarboxylate (2.78 g, 8.03 mmol) was dissolved in acetonitrile (27.1 mL) and water (0.542 mL). Lithium bromide (5.58 g, 64.24 mmol) and triethylamine (4.48 mL, 32.12 mmol) were added and the resulting mixture heated under reflux for 4 h, diluted with Water and MTBE and the organic layer extracted with water. The combined aqueous layers were acidified with 3 M HCl, extracted with MTBE, dried over MgSO4, filtered and evaporated to give 2-(2,4-dichlorophenyl)-1-(methoxy-carbonyl)piperidine-4-carboxylic acid (2.440 g, 91%) as a foam. MS m/z 332 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415378B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-96ec863da0074661b072efff3379791c |
| Source note | uspto-grants-2013_04 |