HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl (cyanomethyl)phosphonate → HCID 69205834, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | HCID 69203625 | HCID 69203625 | — |
| Reactant | 3-(3,5-Dimethoxy-phenyl)-3-(3-methoxy-phenyl)-acrylonitrile | HCID 69205299 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69205834 | HCID 69205834 | 78% |
Reaction Steps
[4-(tert-Butyldimethylsilanyloxy)-3-methoxyphenyl]-(3,5-dimethoxyphenyl)methanone (3.64 g, 9.04 mmol), cyanomethylphosphonic acid diethyl ester (2.85 ml, 18.08 mmol) in anhydrous THF (10 ml), and lithium bis(trimethylsilyl)amide (1.0 M solution in THF, 18.08 ml, 18.08 mmol) were treated in the same manner as described above for the synthesis of 3-(3,5-dimethoxy-phenyl)-3-(3-methoxy-phenyl)-acrylonitrile. The crude was purified via flash column chromatography (5% EtOAc in hexane gradient to 20% EtOAc in hexane in about 30 min.) to give 3-[4-(tert-butyl-dimethyl-silanyloxy)-3-methoxy-phenyl]-3-(3,5-dimethoxy-phenyl)-acrylonitrile as a white solid (3.00 g, 78%). The product was carried over to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07312241B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-3b276ede4475481aa5939a83d2d3d849 |
| Source note | uspto-grants-2007_12 |