HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 6-Bromo-4-methyl-1,4-benzoxazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 6-Bromo-2H-1,4-benzoxazin-3(4H)-one | HCID 16218142 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-Bromo-4-methyl-1,4-benzoxazin-3-one | HCID 53217383 | — |
Reaction Steps
Sodium hydride (0.10 g, 2.6 mmol) was added to a solution of 6-bromo-2H-1,4-benzoxazin-3(4H)-one (0.49 g, 2.1 mmol) in N,N-dimethylformamide (3 mL) under nitrogen. After the mixture was stirred at r.t. for 10 min, methyl iodide (0.27 mL, 4.3 mmol) was added. The reaction mixture was stirred at r.t. for 1 h. Then 10 mL of water was added to the mixture, and a white precipitate was removed by filtration, washed with water, and dried under vacuum to afford the product which was directly used in next step reaction without further purification. LCMS (M+H)+=242.2/244.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266892B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-4860fe20bc02423f80af4e193de3b613 |
| Source note | uspto-grants-2016_02 |