HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine hydrochloride → HCID 22167082, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | 3-Chloro-2,2-dimethylpropanoyl chloride | HCID 61345 | — |
| Reactant | 2-Hydrazinopyridine | HCID 78645 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 22167082 | HCID 22167082 | 71.2% |
Reaction Steps
2-Pyridylhydrazine (10.9 g) in dichloromethane (120 ml) and dry triethylamine (28 ml) were chilled in an ice bath. -β-chloropivaloyl chloride (15.5 g) in dichloromethane (20 ml) was added dropwise with stirring for 15 minutes and the mixture was refluxed for 3 hours. When cool the triethylamine hydrochloride was filtered off and the filtrate evaporated to dryness and rinsed four times with the minimum quantity of ether to give the title compound (13.6 g) after recrystallisation from cyclohexane mp 141°-144°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04824859 |
| Source dataset | uspto-grants-1989_04 |
| ORD ID | ord-e7c363d37e0f4ccabd78f2c9f5bf69c8 |
| Source note | uspto-grants-1989_04 |