HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pentaerythritol → (1-Methyl-2,6,7-trioxabicyclo[2.2.2]octan-4-yl)methanol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pentaerythritol | HCID 8285 | — |
| Edukt | Triethyl orthoacetate | HCID 66221 | — |
| Edukt | Pyridine 4-methylbenzene-1-sulfonate | HCID 161440 | — |
| Lösungsmittel | di-N-Octyl Phthalate | HCID 8346 | — |
| Produkt | (1-Methyl-2,6,7-trioxabicyclo[2.2.2]octan-4-yl)methanol | HCID 13547990 | 85% |
Reaktionsschritte
Pentaerythritol (13.6 g, 0.1 mol), triethyl orthoacetate (16.22 g, 0.1 mol, 18.3 mL), pyridine p-toluenesulfonate (PPTS) (0.5 g, 2 mmol) and 100 mL of dioctyl phthalate were mixed in a 250 mL, round-bottom flask fitted with a regular distillation apparatus. The mixture was heated to 130°-140° C. and ethanol was slowly distilled. When the amount of ethanol was close to the theoretical value the pressure was reduced to <0.1 torr and the product was distilled in vacuo. The white product which distilled crystallized in the condenser to give 13.6-14.9 g of MHTBO. Yield: 85-93%. The compound can be recrystallized from toluene but can be used directly. Mp: 110°-112° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05478924 |
| Quelldatensatz | uspto-grants-1995_12 |
| ORD ID | ord-888103a365844a97931382d5cab0ce23 |
| Quellennotiz | uspto-grants-1995_12 |