HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-methyl-8-nitro-2H-1,4-benzoxazin-3(4H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 8-Nitro-2H-benzo[B][1,4]oxazin-3(4H)-one | HCID 38997184 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-methyl-8-nitro-2H-1,4-benzoxazin-3(4H)-one | HCID 38997176 | — |
Reaction Steps
Sodium hydride (60%) (300 mg, 7.50 mmol) was added to a solution of 8-nitro-2 H-1,4-benzoxazin-3(4 H)-one (971 mg, 5.00 mmol) in N,N-dimethylformamide (15 mL) at room temperature, the mixture was stirred for 10 min, and then methyl iodide (374 μL, 6.00 mmol) was added dropwise thereto. The mixture was stirred at room temperature for 3 hr and water was added to the reaction mixture. The resulting precipitate was collected by filtration, washed with ethyl acetate and water, and then dried at 60° C. under reduced pressure to afford 4-methyl-8-nitro-2 H-1,4-benzoxazin-3(4 H)-one as a pale yellow amorphous substance (453 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09035059B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-186321116b2e44dc91fadf96bd7afeb6 |
| Source note | uspto-grants-2015_05 |