HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 66646046, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 66645913 | HCID 66645913 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66646046 | HCID 66646046 | 80% |
Reaction Steps
A dichloromethane solution (36 ml) of 2M boron tribromide was added dropwise to a dichloromethane solution of 6-methoxy-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (5.0 g, 26 mmol) under ice cooling and the mixture was stirred overnight. Water was added to the reaction solution to decompose the reagents excessively present. The reaction solution was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1). The purified product was concentrated to dryness under reduced pressure to obtain 6-hydroxy-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (4.02 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071600B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-614f0a2e258444a788a94da37251c5dc |
| Source note | uspto-grants-2011_12 |