HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337041 | — |
| Solvent | Benzene ethyl acetate | HCID 21583983 | — |
| Product | 2-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin | HCID 12687125 | 85% |
Reaction Steps
An amount of 1.7g of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin was dissolved in 50ml of anhydrous ethanol and the mixture was refluxed for 3 hours, while hydrogen chloride gas was bubbled into the mixture. The solvent was distilled off to obtain the residue which was dissolved in the mixed solvent of ethyl acetate-benzene. The solution was washed with saturated sodium chloride solution and freed of solvent by distillation to obtain 1.6g (85%) of 2-hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 125°-129° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04101667 |
| Source dataset | uspto-grants-1978_07 |
| ORD ID | ord-20dd8bc6d435451bb30eb9aed3574b35 |
| Source note | uspto-grants-1978_07 |