HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Ethyl 2-methyl-3-(4-methylphenyl)-2-propenoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Methylbenzaldehyde | HCID 7725 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Triethyl 2-phosphonopropionate | HCID 107155 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Ethyl 2-methyl-3-(4-methylphenyl)-2-propenoate | HCID 68712312 | 91% |
Reaction Steps
To a suspension of sodium hydride (a 60% dispersion in liquid paraffin, 15.0 g, 375 mmol) in N,N-dimethylformamide (160 ml) was added at 0° C. a solution of triethyl 2-phosphonopropionate (87.7 g, 368 mmol) in N,N-dimethylformamide (10 ml) and the resulting mixture was stirred at the same temperature for 1 hour. To the reaction solution was added 4-methylbenzaldehyde (43.3 g, 361 mmol) and the resulting mixture was stirred at room temperature for 1 hour. Water was added into the reaction solution and the product was extracted twice with ethyl acetate. The combined extracts were washed with water, dried on magnesium sulfate, and then concentrated under reduced pressure to obtain 66.7 g (91% yield) of the oily title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07101867B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-3639eb7d53bf48209d262eadb940099a |
| Source note | uspto-grants-2006_09 |