HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (2,6-Difluoro-4-methoxy-phenyl)-hydrazine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Di-tert-butyl 1-(2,6-difluoro-4-methoxyphenyl)hydrazine-1,2-dicarboxylate | HCID 68157167 | — |
| Product | (2,6-Difluoro-4-methoxy-phenyl)-hydrazine hydrochloride | HCID 68156785 | — |
Reaction Steps
Di-tert-butyl 1-(2,6-difluoro-4-methoxyphenyl)hydrazine-1,2-dicarboxylate (616 mg, 1.64 mmol) was heated in 4 M HCl in dioxane (5 mL, 20 mmol) at reflux. The solution over time became a suspension. At 30 min, the reaction was cooled, diethylether was added, and the solid was collected with a medium frit, washing with diethylether. This gave (2,6-difluo-4-methoxy-phenyl)-hydrazine hydrochloride (0.246 g, 86%) as a tan solid. 1H NMR (400 MHz, DMSO-d6, δ): 9.75 (br. s., 3H) 7.46 (s, 1H) 6.79-6.90 (m, 2H) 3.78 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859591B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-394619cb18b34fa882f6f25faba269af |
| Source note | uspto-grants-2014_10 |