HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Propanol → HCID 12521033, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Propanol | HCID 1031 | — |
| Edukt | Phosphorodichloridothioic acid, O-ethyl ester | HCID 73907 | — |
| Edukt | 1-Propanol, sodium salt | HCID 23669363 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 12521033 | HCID 12521033 | 59,1% |
Reaktionsschritte
To 30 g (167 mmole) of O-ethyl dichlorothiophosphate in 100 ml of tetrahydrofuran (THF) and cooled to -70° C. was added a solution of sodium propoxide (from 7.4 g of 60% NaH (184 mmole) and 11 g (176 mmole) of 1-propanol) in 50 ml of THF. After warming to room temperature over 2 hours, the THF was removed in vacuo and the residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water. The organic layer was dried over magnesium sulfate, concentrated in vacuo, and distilled (bp 45°-50° C. 1 torr) yielding 20 g of the title compound, an oil. nmr 1.0 t 3H, 1.4 t 3H, 1.8 sextet 2H, 4.4M 4H.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05536711 |
| Quelldatensatz | uspto-grants-1996_07 |
| ORD ID | ord-ed45dc17f2de4ca7a18e85bc18e09f7c |
| Quellennotiz | uspto-grants-1996_07 |