HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 20290836, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 20290820 | HCID 20290820 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 20290836 | HCID 20290836 | — |
Reaction Steps
to a solution of 2,3-dihydro-7-methyl-9-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]-5H-pyrido[1,2,3-de]-1,4-benzoxazin-5-one in dimethylformamide is added sodium hydride and dimethyl sulfate. The solution is stirred for 24 hours, treated with ethanol and added to water. The resultant recipitate is filtered, triterated with 10% sodium hydroxide solution and filtered. The residual solid is recrystallized to give 2,3-dihydro-7-methyl-9-[2,2,2-trifluoro-1-methoxy-1-(trifluoromethyl) ethyl]-5H-pyrido[1,2,3-de]-1,4-benzoxazin-5-one. If desired sodium hydride may be replaced by a base such as potassium carbonate or potassium t-butoxide and dimethyl sulfate may be replaced by methyl iodide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04251534 |
| Source dataset | uspto-grants-1981_02 |
| ORD ID | ord-ea0af21fdece4c85b63eab0d966ad75f |
| Source note | uspto-grants-1981_02 |