HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15429393, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | (2,4,6-Trichlorophenyl)hydrazine | HCID 79234 | — |
| Reactant | Butanoic acid, 2-[bis(methylthio)methylene]-3-oxo-, ethyl ester | HCID 4997384 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 15429393 | HCID 15429393 | 56.4% |
Reaction Steps
A mixture of 1.22 g (5.23 mmol) of ethyl 3,3-bismethylthio-2-acetylacrylate and 1.11 g (5.23 mmol) of 2,4,6-trichlorophenylhydrazine in 12 mL of ethanol was heated at reflux for 2 hours. The cooled reaction mixture was then poured into cold water and the product was extracted into ether. The ethereal extracts were dried and evaporated and the residues were chromatographed on silica gel using 6:1 hexane/ethyl acetate as eluent to give 1.12 g (56%) of the desired product as a crystalline solid, m.p. 95-98° C. 1H-NMR (CDCl3) δ1.38 (3H, t, J=7), 2.30 (3H, s), 2.49 (3H, s.), 4.31 (2H, q, J=7), 7.47 m(2H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05958948 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-b7e4380c81fe49beaf59490dd05c6b2b |
| Source note | uspto-grants-1999_09 |