HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 20271482, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 20255500 | HCID 20255500 | — |
| Reactant | HCID 178418287 | HCID 178418287 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 20271482 | HCID 20271482 | 106.4% |
Reaction Steps
Dissolve 568 mg (2.2 mmole) of 2-fluoro-7-hydroxymethyldibenzo[b,f]thiepin in 30 ml of methylene chloride and add 647 mg of 98% pyridinium chlorochromate. Stir the mixture and follow the reaction by thin layer chromatography (Merck silica gel F254 with 5% ethyl acetate in toluene). When complete, filter the mixture through a bed of Florisil, and wash through with methylene chloride. Evaporate the filtrate to obtain a brown solid (600 mg). Purify the crude product by chromatography on silica gel using totluene as solvent to obtain the title compound as a yellow solid, m.p. 137°-139° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04535171 |
| Source dataset | uspto-grants-1985_08 |
| ORD ID | ord-a128d188c8c246948ad06dae625d4703 |
| Source note | uspto-grants-1985_08 |