HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 7-(4-Trifluoromethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl 7-(4-trifluoromethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate | HCID 21995679 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 7-(4-Trifluoromethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid | HCID 21995950 | 75.9% |
Reaction Steps
To a solution of methyl 7-(4-trifluoromethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) in 1,2-dimethoxyethane (40 ml) was added at room temperature 6N hydrochloric acid (20 ml), and the mixture was refluxed for 22 hours, cooled to room temperature and extracted with ethyl acetate/THF. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give crystals, which were collected by filtration. The crystals were washed with hexane to give colorless crystals of 7-(4-trifluoromethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (439.5 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235771B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-6a645d6889e345418baef8cd0ad62327 |
| Source note | uspto-grants-2001_05 |