HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → 3-(2-Nitro-benzo[d]phenyl)-2-methyl-2-propenoic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 3-Nitro-2-naphthaldehyde | HCID 12069028 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Product | 3-(2-Nitro-benzo[d]phenyl)-2-methyl-2-propenoic acid ethyl ester | HCID 70214934 | — |
Reaction Steps
To 200 ml of benzene, 9.3 g (46 mmol) of 3-nitro-2-naphtaldehyde and 17.6 g (48.5 mmol) of Wittig reagent (carbethoxy ethylidene triphenylphosphorane) (manufactured by Aldrich Chemical Co., Inc.) were added, and the resulting mixture was stirred at room temperature for one night. The completion of the reaction was verified by TLC, and the reaction liquid was concentrated, whereby a crude product was obtained. This crude product was refined by a column chromatography (aminopropyl-modified silica gel (Fuji Silysia Chem. Co., NH-DM); developing solvent: hexane/ethyl acetate=1/1), whereby 13.0 g of the aimed compound were obtained as a crystal (yield: 96%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329546B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-1d913e397ccf4b999d44b84f7cb27897 |
| Source note | uspto-grants-2001_12 |