HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methylbenzaldehyde → Ethyl 3-methylcinnamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methylbenzaldehyde | HCID 12105 | — |
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Reactant | Ethyl [bis(2,2,2-trifluoroethoxy)phosphinyl]acetate | HCID 11759356 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 3-methylcinnamate | HCID 589327 | — |
Reaction Steps
KHMDS (4.0 g, 20.0 mmol) was added to a solution of ethyl[bis(2,2,2-trifluoro-ethoxy)phosphinyl]acetate (4.7 mL, 20.0 mmol) and 18-crown-6 (10.6 g, 40.0 mmol) in THF (200 mL) at −78° C., and stirred for 30 minutes. m-Tolualdehyde (2.1 mL, 18 mmol) was added and the reaction mixture was stirred for 3 hours from −78° C. to room temperature. The reaction was quenched with aqueous hydrochloric acid (1 M solution, 100 mL), and the product was extracted with EtOAc (3×100 mL). The organic extracts were washed with brine (100 mL), dried over MgSO4, and concentrated to afford the subtitle compound, which was used without further purification. MS calculated for C12H14O2+H: 191, observed: 191.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08232311B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-b69f022a9b6d4f8ca8a0302ee404d34d |
| Source note | uspto-grants-2012_07 |