HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23355188, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,1-Bis(methylthio)-2-nitroethylene | HCID 83623 | — |
| Reactant | HCID 23355179 | HCID 23355179 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 23355188 | HCID 23355188 | 85.2% |
Reaction Steps
A solution of 2-amino-2',5-dichlorobenzophenone hydrochloride (1.6 g, 5.3 mmol) and 1,1-bis(methylthio)-2-nitroethylene (875 mg, 5.3 mmol) in 12 ml acetic acid was heated at 120° C. overnight. The reaction mixture was cooled to room temperature, 30 ml of water was added and the resulting mixture was extracted with 2×60 ml ethyl acetate. The ethyl acetate extracts were washed with 2×50 ml water, 2×50 ml saturated sodium bicarbonate solution and 50 ml brine, and then dried (anhydrous sodium sulfate), filtered and concentrated in vacuo. The residue was chromatographed on silica gel (440 g, 230-400 mesh), eluting with 85:15 hexane/ethyl acetate to yield the title compound as a yellow solid (1.65 g, 72% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05596001 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-4b868d0f107941afbf95a6a25500e8cb |
| Source note | uspto-grants-1997_01 |