HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 117702704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 22372393 | HCID 22372393 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 117702704 | HCID 117702704 | 95.3% |
Reaction Steps
To a suspension of 2-hydrazinyl-3-methoxy-5-nitropyridine (Step 84.1) (20 g, 106 mmol) in dioxane (170 mL) was added at RT Ac2O (13.1 mL, 138 mmol) and the reaction mixture was stirred for 1 hr at RT. The reaction mixture was poured onto ice-water (700 mL) 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 (23.3 g, 101 mmol, 95% yield) as a yellow solid. tR: 0.45 min (LC-MS 2); ESI-MS: 227 [M+H]+ (LC-MS 2); ESI-MS: 225 [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-2dff954ca0b54a19b5193bdd040f3d44 |
| Source note | uspto-grants-2015_03 |