HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23317901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Crotonaldehyde | HCID 447466 | — |
| Reactant | HCID 86740835 | HCID 86740835 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 23317901 | HCID 23317901 | 92% |
Reaction Steps
To a solution of 4-phenylbutyl phosphonous acid, ethyl ester (0.5 g, 0.0022 mole) in chloroform (15 ml) was added triethylamine (0.34 ml, 0.0024 mole), trimethyl silylchloride (0.30 ml, 0.0024 mole) and crotonaldehyde (0.20 ml, 0.0024 mole). The reaction mixture was stirred at reflux temperature for 18 hours; the mixture was poured into crushed ice (15 gm) containing 10 ml 5% HCl acid. It was shaken in a separatory funnel; a chloroform layer was evaporated, and the aqueous layer extracted once with 20 ml chloroform. The combined organic phase was washed with water, dried over anhydrous sodium sulphate and the organic solvent removed on a rotavap to produce the title compound as a yellow oil (0.60 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04594199 |
| Source dataset | uspto-grants-1986_06 |
| ORD ID | ord-33639d3156bf4c0ba4e9dd1ec70d5b78 |
| Source note | uspto-grants-1986_06 |