HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → HCID 68862086, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Ethyl orthoformate | HCID 31214 | — |
| Edukt | Propanediol | HCID 134919 | — |
| Edukt | 2,6-Dibromobenzaldehyde | HCID 12648641 | — |
| Katalysator | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 68862086 | HCID 68862086 | 98% |
Reaktionsschritte
2,6-Dibromobenzaldehyde (49) (10.0 g, 37.9 mmol) was dissolved in 160 ml dry CH2Cl2. Propanediol (6.4 ml, 88.5 ml), triethylorthoformate (6.83 ml, 41 mmol) and anhydrous ZrCl4 (1.0 g) were added at ambient temperature and stirred overnight. Then NaOH (50 ml of a 10% solution) was added and stirred for an additional hour. The organic phase was separated, the aqueous phase was extracted with Et2O (2×40 ml). The combined organic phases were washed with water (3×60 ml), dried over MgSO4 and the volatiles were removed in vacuo to afford 12 g (98%) 2-(2,6-Dibromophenyl)-1,3-dioxane (acetal) as a slightly yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08969624B2 |
| Quelldatensatz | uspto-grants-2015_03 |
| ORD ID | ord-39a49ebe1c9f419c8d447ac9182f1073 |
| Quellennotiz | uspto-grants-2015_03 |