HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57927199, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Epibromohydrin | HCID 18430 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3H-1,2,4-Triazol-3-one, 2,4-dihydro-4,5-dimethyl- | HCID 143196 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57927199 | HCID 57927199 | — |
Reaction Steps
After dissolving 4,5-dimethyl-2,4-dihydro[1,2,4]triazol-3-one (CAS 54770-19-3) (560 mg) in N,N-dimethylformamide (5 ml), sodium hydride (60% in oil) (238 mg) and epibromohydrin (0.85 ml) were added and the mixture was stirred at room temperature for one day. Water was added to the reaction mixture, and extraction was performed with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (390 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08252810B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-911cbfdb9db540a09b71ae4100751109 |
| Source note | uspto-grants-2012_08 |