HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl pyruvate → Methyl 2-Methyl-5,5-diphenyl[1,3]dioxane-2-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl pyruvate | HCID 11748 | — |
| Edukt | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Edukt | 2,2-Diphenylpropane-1,3-diol | HCID 410445 | — |
| Produkt | Methyl 2-Methyl-5,5-diphenyl[1,3]dioxane-2-carboxylate | HCID 15428822 | 22,4% |
Reaktionsschritte
A mixture of 22.8 g (0.1 M) of 2,2-diphenyl-1,3-propanediol and 100 g (0.98 M) of methyl pyruvate is brought to 70° C. in a 500 ml round-bottomed flask under a nitrogen atmosphere. 22.4 g (0.156 M) of P2O5 are added portionwise. An exothermic reaction takes place and the temperature rises to 98° C. The mixture is allowed to return to room temperature and is poured slowly into ice-cold water. This mixture is extracted with methylene chloride and the extracts are washed with sodium hydroxide and water. The extracts are concentrated and the residue is chromatographed by flash chromatography (70 CH2Cl2/50 cyclohexane eluent). The product is then recrystallized from 40 ml of diisopropyl ether. 7 g of a product of m.p. 116° C. are obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06528538B1 |
| Quelldatensatz | uspto-grants-2003_03 |
| ORD ID | ord-d44e178896d34d1297817129dfb18f97 |
| Quellennotiz | uspto-grants-2003_03 |