HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-METHYLACETOPHENONE → HCID 66749100, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-METHYLACETOPHENONE | HCID 8500 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66749100 | HCID 66749100 | — |
Reaction Steps
To a solution of diethyl cyanomethylphosphonate (13.2 g, 74.6 mmol) in 50 mL of THF was added sodium hydride (60% content, 2.98 g, 74.6 mmol). The mixture was stirred at room temperature for 2 hours. 1-(4-methylphenyl)ethanone (5 g, 37.3 mmol) was added and the mixture was stirred for 2 hours. After evaporation of THF, the residue was taken up in ethyl acetate (50 mL) and quenched with water (50 mL). The organic phase was washed with water (50 mL), dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo, and the residue was used in the next step without further purification. LC-MS: m/z 158 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156788B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-f31ec644165d4b1b9e16c10dfda87388 |
| Source note | uspto-grants-2015_10 |