HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68537407, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-4-methyl-5-nitropyridine | HCID 345364 | — |
| Reactant | HCID 68540093 | HCID 68540093 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68537407 | HCID 68537407 | — |
Reaction Steps
Stir a solution of 2-chloro-4-methyl-5-nitro-pyridine (0.85 mmol, 0.15 g), 2,2-dimethyl-1-piperazin-1-yl-propan-1-one hydrochloride (0.94 mmol, 0.16 g) and triethylamine (2.12 mmol, 0.3 mL) in a sealed tube at 80° C. overnight. Cool down the mixture to room temperature, add CH2Cl2 and wash with saturated aq. sodium chloride. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give 2,2-dimethyl—[4-(4-methyl-5-nitro-pyridin-2-yl)-piperazin-1-yl]-propane-1-one. Subject residue to silica gel chromatography eluting with hexanes/ethyl acetate in a gradient (from 30% up to 60%). MS(ES): m/z=307 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652015B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-d9ba5287425e490fa1bbcccd1b6ca5ac |
| Source note | uspto-grants-2010_01 |