HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazinium chloride → Ethyl 6-(2-ethylaminopyrimidin-4-yl)-3-oxo-2,3-dihydropyridazine-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazinium chloride | HCID 115031 | — |
| Reactant | Diethyl 2-[2-(2-ethylaminopyrimidin-4-yl)-2-oxo-ethyl]-2-hydroxymalonate | HCID 68452836 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 6-(2-ethylaminopyrimidin-4-yl)-3-oxo-2,3-dihydropyridazine-4-carboxylate | HCID 68453190 | — |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
A mixture of 2 g of diethyl 2-[2-(2-ethylaminopyrimidin-4-yl)-2-oxo-ethyl]-2-hydroxy-malonate, 485 mg of hydrazine hydrochloride and 20 ml of ethanol is stirred under reflux for 24 hours. After cooling while stirring, the precipitate is filtered off with suction, heated in 4 ml of N-methylpyrrolidinone (NMP) at 130° C. for 3 hours and, after cooling, mixed with 15 ml of n-heptane and stirred. The precipitate is then filtered off with suction and stirred with methylene chloride, again filtered off with suction and dried.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07727989B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-d8366a1b2fef4b479476f79a57cde650 |
| Source note | uspto-grants-2010_06 |