HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 66991737, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | tert-Butyl diethylphosphonoacetate | HCID 2773685 | — |
| Reactant | HCID 86619746 | HCID 86619746 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66991737 | HCID 66991737 | 84.2% |
Reaction Steps
2-methoxy-4-(3-oxo-3-phenyl-propenyl)-benzaldehyde (550 mg, 2.07 mmol) was dissolved in THF (5 ml) and the resulting solution was added to a stirring mixture of tert-butyl diethylphosphonoacetate (603 mg, 2.27 mmol) and NaH (107 mg, 2.69 mmol, 60% oil dispersion) in THF (5 ml). After 15 minutes the reaction was quenched by the addition of water and partitioned between water and EtOAc. The organic extract was dried over Na2SO4 and evaporated under vacuo giving a crude that was purified by silica gel chromatography (EtOAc/petroleum ether 1:6). The collected fraction gave 635 mg of 3-[2-methoxy-4-(3-oxo-3-phenyl-propenyl)-phenyl]-acrylic acid tert-butyl ester as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058273B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-c47d5252913243d3b0723fe9cc085630 |
| Source note | uspto-grants-2011_11 |