HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → 1-(6-Chloro-2-pyrazinyl)-4,5-dihydro-5-methyl-1H-pyrazol-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Crotononitrile | HCID 637921 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | 2-Chloro-6-hydrazinylpyrazine | HCID 12693185 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 1-(6-Chloro-2-pyrazinyl)-4,5-dihydro-5-methyl-1H-pyrazol-3-amine | HCID 20228182 | — |
Reaction Steps
A 0.30 g. amount of sodium metal is dissolved in 100 ml. of absolute ethanol, then 6.72 g. of 2-chloro-6-hydrazinopyrazine (prepared as described above) is added and after 5 minutes, 4.6 g. of distilled crotononitrile is added. The reaction mixture is refluxed for 6 hours. The solvent is removed in vacuo and water is added to the residue to separate a gum. The gum is dissolved in dichloromethane, dried over magnesium sulfate and filtered. The filtrate is evaporated to give a gum. The gum is treated with benzene to separate yellow crystals. The crystals are collected, dried and recrystallized from acetone-hexane to give 1.4 g of the desired product as yellow crystals, m.p. 147°-148° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04622401 |
| Source dataset | uspto-grants-1986_11 |
| ORD ID | ord-24bace7734ec424abb0bc091444b3d16 |
| Source note | uspto-grants-1986_11 |