HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trimethylolpropane → 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trimethylolpropane | HCID 6510 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1,1-Dimethoxyethane | HCID 10795 | — |
| Katalysator | Diammonium molybdate | HCID 61578 | — |
| Katalysator | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl- | HCID 11816152 | 95% |
Reaktionsschritte
Trimethylolpropane (10.0 g; 74.6 mmol), 2,2-dimethoxyethane (9.01 g; 86.5 mmol) and p-toluenesulfonic acid monohydrate (0.369 g; 1.94 mmol) were dissolved in tetrahydrofuran (125 mL). The clear solution was stirred at ambient temperature for 24 h. TLC (stained with ammonium molybdate) confirmed near quantitative conversion of the starting triol. The reaction was neutralised with triethylamine (10 mL) and all volatiles were removed in vacuo. Colourless oily residue was passed through a silicagel column (eluent ethyl acetate/cyclohexane 1:1). The eluent was evaporated to provide (5-ethyl-2,2-dimethyl-1,3-dioxan-5-yl)methanol (12.34 g; 95% yield) as a colourless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09296835B2 |
| Quelldatensatz | uspto-grants-2016_03 |
| ORD ID | ord-36b3516933c442f9b5823fb96a670468 |
| Quellennotiz | uspto-grants-2016_03 |