HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 178424217, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 2-(2-Methylbenzyl)-3-oxobutanenitrile | HCID 86724886 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178424217 | HCID 178424217 | 38% |
Reaction Steps
To a solution of 2-(2-methylbenzyl)-3-oxobutanenitrile (7.39 g, 39.5 mmol) in ethanol (400 mL) was added hydrazine hydrate (1.97 g, 39.5 mmol) and stirred under reflux for 16 h. The mixture was cooled to room temperature and concentrated. The residue was purified by silica gel column (petroleum ether/ethyl acetate=1/1 then DCM:methanol=40:1) to provide the titled compound (3.005 g, 38%) as a yellow solid; LC/MS: MS (ES+) m/e 202 (MH+); 1H NMR (300 MHz, CDCl3) δ ppm 2.12 (s, 3H), 2.33 (s, 3H), 3.63 (s, 2H), 7.07-7.17 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096605B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-518e79a1ec9140d0ac67ff96af27ceec |
| Source note | uspto-grants-2015_08 |