HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 178470096, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Diethyl [(2,3,4-trifluoroanilino)(p-methoxybenzylthio)methylene]malonate | HCID 14673304 | — |
| Solvent | Diphenyl Ether | HCID 7583 | — |
| Product | HCID 178470096 | HCID 178470096 | 82.1% |
Reaction Steps
A solution of diethyl [(2,3,4-trifluoroanilino)(p-methoxybenzylthio)methylene]malonate (80.9 g) in diphenyl ether (60 ml) heated at 110° C. was added dropwise to diphenyl ether (210 ml) kept at 250° to 260° C. with stirring under nitrogen stream over a period of 15 minutes. After the reaction mixture was further stirred at the same temperature for 5 minutes, the mixture was cooled to room temperature and added to hexane (3000 ml). The resulting precipitate was filtered to give the title compound (59.9 g), which was recrystallized from ethyl acetate to give yellow crystals, m.p. 174°-176° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04808584 |
| Source dataset | uspto-grants-1989_02 |
| ORD ID | ord-c03cd15341cd4ef39702a69729f99682 |
| Source note | uspto-grants-1989_02 |