HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → Ethyl 3-(4-chloro-2-nitrophenyl)-2-methyl-2-propenate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 4-Chloro-2-nitrobenzaldehyde | HCID 79674 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Product | Ethyl 3-(4-chloro-2-nitrophenyl)-2-methyl-2-propenate | HCID 70214465 | — |
Reaction Steps
Into 200 ml of benzene, 10.0 g (53.8 mmol) of 4-chloro-2-nitrobenzaldehyde (manufactured by Aldrich Chemical Co., Inc.) and 18.1 g (50.0 mmol) of Wittig reagent (carbethoxyethylidene triphenylphosphorane, manufactured by Aldrich Chemical Co., Inc.) were dissolved; and the mixture was stirred at ordinary temperature for one night. After the completion of the reaction was verified by TLC, 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 13.1 g of the aimed compound were obtained as a crystal (yield: 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06229020B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-db699a6678f14001ae6990c9d9748df8 |
| Source note | uspto-grants-2001_05 |