HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → (E)-methyl 3-[3-(methylcarbamoyl)phenyl]prop-2-enoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester | HCID 17453 | — |
| Reactant | 3-formyl-N-methylbenzamide | HCID 22051433 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (E)-methyl 3-[3-(methylcarbamoyl)phenyl]prop-2-enoate | HCID 66589796 | 97% |
Reaction Steps
A solution of 3-formyl-N-methylbenzamide (2.9 g, 17.77 mmol) and methyl 2-triphenylphosphoranylideneacetate (8.91 g, 26.66 mmol) in dichloromethane (85 mL), was stirred at room temperature for 18 h. The reaction mixture was evaporated to dryness. The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 10% MeOH in DCM. Pure fractions were evaporated to dryness to afford impure product. Re-purified by silica column chromatography, eluting with a gradient of 50 to 100% EtOAc in hexanes. Pure fractions were evaporated to dryness to afford (E)-methyl 3-[3-(methylcarbamoyl)phenyl]prop-2-enoate (3.77 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08129391B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-ae3fad8ddc284bf79623f6ef6eee32f3 |
| Source note | uspto-grants-2012_03 |