Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl bromide | HCID 10482 | — |
| Reactant | 5-Methoxy-2-methyl-4-nitropyridine 1-oxide | HCID 15163457 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 86703139 | HCID 86703139 | — |
Reaction Steps
5-Methoxy-2-methyl-4-nitro-pyridine-1-oxide (Step AL5) (1.9 g, 10.3 mmol) and acetyl bromide (22.9 mL, 310 mmol) was added to acetic acid (40 mL) and the reaction was stirred at 80° C. for 1 h. The mixture was concentrated (1/3) and a solution of NaOH was added. The resulting mixture was extracted with EtOAc, washed with brine, dried (Na2SO4), filtered and concentrated. The product was crystallised (EtOAc/TBME). ESI-MS: tR=0.54 min, [M+H]+ 218.1/220.1 (LC-MS 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09365576B2 |
|---|
| Source dataset | uspto-grants-2016_06 |
|---|
| ORD ID | ord-f96c31e4869147be9d38b9522a6a9647 |
|---|
| Source note | uspto-grants-2016_06 |
|---|