HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 18688666, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 18688662 | HCID 18688662 | — |
| Product | HCID 18688666 | HCID 18688666 | — |
Reaction Steps
Methyl 2-(10,11-dihydro-1i-methoxycarbonyl-10-oxodibenzo[b,f]thiepin-2-yl)propionate (prepared in Example 22, 18 mg, 0.040 mmol.), acetic acid (0.3 mL) and 6N hydrochloric acid (0.3 mL) were mixed, and the mixture was heated for 2 hours under reflux. To the reaction mixture was added water, and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate portion was washed successively with water and an aqueous saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The dried ethyl acetate portion was placed under reduced pressure to distill the solvent off. The residue was dissolved in toluene and concentrated under reduced pressure to give 14 mg of the desired compound as a white crystalline product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06111115 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-21f1231ee96e4a5f9cdcf2a5c59704b7 |
| Source note | uspto-grants-2000_08 |