HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 22118326, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22118311 | HCID 22118311 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22118326 | HCID 22118326 | — |
Reaction Steps
Sodium hydride (67 mg of 60%) was added to a stirred solution of ethyl 4-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,4-dimethyl-3-oxo-pentanoate (0.4 g) in N,N-dimethylformamide at 0° C. lodomethane (0.1 ml) was added and stirring continued for 16 hours. Ether was added and the organic phase washed (brine), dried (magnesium sulphate), evaporated and the residue purified by column chromatography eluting with ethyl acetate/hexane (1:2) to give ethyl 4-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2,2,4-trimethyl-3-oxo-pentanoate (Compound 197, 0.3 g), NMR 1.21(3H, t), 1.47(6H, s), 1.52(6H, s), 1.92(3H, s), 4.13(2H, q), 5.16(2H, s), 7.2-7.4(5H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06159902 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-248b294f383340229e841956a512beba |
| Source note | uspto-grants-2000_12 |