HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → N'-(3-methyl-5-nitropyridin-2-yl)acetohydrazide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 2-Hydrazinyl-3-methyl-5-nitropyridine | HCID 4236132 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | N'-(3-methyl-5-nitropyridin-2-yl)acetohydrazide | HCID 84818704 | 100% |
Reaction Steps
To a suspension 2-hydrazinyl-3-methyl-5-nitropyridine (Step 67.1) (33.2 g, 198 mmol) in dioxane (175 mL) was added Ac2O (20.5 mL, 217 mmol) and the reaction was stirred at RT for min. The reaction mixture was poured onto ice-water and stirred for 1 hr at 0° C. The precipitate was collected by filtration, washed with H2O and Et2O, and dried under reduced pressure at 50° C. to afford the title product (41.5 g, 198 mmol, 99.5% yield) as light beige solid. tR: 0.45 min (LC-MS 2); ESI-MS: 211 [M+H]+; ESI-MS: 209 [M−H]− (LC-MS 2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975417B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-09bdcfece15d45468ded2e7d9a311ac3 |
| Source note | uspto-grants-2015_03 |