HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethylpentan-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethylpentan-3-ol | HCID 18795530 | — |
| Reactant | HCID 178418287 | HCID 178418287 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethylpentan-3-one | HCID 18795478 | 49.7% |
Reaction Steps
A solution of 2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethylpentan-3-ol (1.7 g) in dichloromethane was added to a stirred mixture of pyridinium chlorochromate (1.81 g) and powdered molecular sieve (4A) in dichloromethane at 20° C. After 5 hours, ether was added, the mixture filtered through hyflo and evaporated. The residue was purified by dry column chromatography on silica gel, eluting with dichloromethane/ethyl acetate to give 2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethylpentan-3-one (Compound 1, 0.84 g) as a white solid, m-p. 98.6-101.6° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06046135 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-1d0ce245f19c45618819c65e0fc4c1ca |
| Source note | uspto-grants-2000_04 |