HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 86696525, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 86696524 | HCID 86696524 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86696525 | HCID 86696525 | 101.3% |
Reaction Steps
A mixture of 2-chloro-N-(((1S,2S)-2-(4-fluorophenyl)cyclopropyl)methyl)-3-(trifluoromethyl)pyridin-4-amine (0.7 g, 2.031 mmol) and hydrazine monohydrate (2.033 g, 40.6 mmol) in dioxane (8 mL) was heated to reflux under nitrogen for 16 h. The reaction mixture was diluted with EtOAc and extracted with aqueous sodium bicarbonate. The aqueous layer was extracted with EtOAc (2×5 mL). The combined organic layers were washed with aqueous sodium bicarbonate (10 mL) and brine (10 mL), dried over magnesium sulfate, filtered and concentrated under vacuum to give N-(((1S,2S)-2-(4-fluorophenyl)cyclopropyl)methyl)-2-hydrazinyl-3-(trifluoromethyl)pyridin-4-amine (0.7 g, 65%) which was used for the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765767B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-0475a41caa0f41c08b54c136a9028114 |
| Source note | uspto-grants-2014_07 |