HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → methyl 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Methyl 2-methoxycarbonylmethyloxyphenoxyacetate | HCID 347859 | — |
| Reactant | Potassium | HCID 5462222 | — |
| Reactant | Butan-1-olate | HCID 12476378 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | methyl 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin-2-carboxylate | HCID 13544514 | — |
Reaction Steps
Potassium t.-butoxide (15.8 g.) dissolved in DMSO (130 ml.) is added dropwise over a 45 minute period to 1,2-bis-carbomethoxymethoxybenzene (18.3 g.) in DMSO (30 ml.) under an atmosphere of nitrogen. The mixture then is stirred 3 hours at ambient temperature and a mixture of acetic acid (16 ml.) and water (200 ml.) is added. The reaction mixture is extracted with benzene, the powdery material removed by filtration and the benzene then dried over magnesium sulfate and the benzene then evaporated leaving 3-oxo-4-carbomethoxy-3,4-dihydro-2H-1,5-benzodioxepin that is used in the following step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03944560 |
| Source dataset | uspto-grants-1976_03 |
| ORD ID | ord-766110ea60d7478594a1f48108ef4b28 |
| Source note | uspto-grants-1976_03 |