HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69666585, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Methyl 3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylate | HCID 69667024 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69666585 | HCID 69666585 | 63.4% |
Reaction Steps
145 mg (2.6 mmol) of potassium hydroxide pellets are added to 0.5 g (2 mmol) of methyl 3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylate, prepared according to example 32, in solution in 8 ml of 80% aqueous ethanol, and the medium is brought to reflux for 3 hours. After cooling, the medium is brought to acidity by addition of 1N hydrochloric acid. The precipitate is filtered off and then washed with diisopropyl ether to provide 300 mg (63%) of 3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylic acid in the form of a white solid comprising two Z/E isomers as a mixture in an 85/15 ratio; M.p.>260° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07071340B2 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-ec588e9c9ad0476aa2ef0f51fdd2c601 |
| Source note | uspto-grants-2006_07 |