HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → 2,6,7-Trioxabicyclo[2.2.2]octane, 1,4-diethyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Trimethylolpropane | HCID 6510 | — |
| Reactant | Diglyme | HCID 8150 | — |
| Reactant | Ethyl orthopropionate | HCID 66995 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2,6,7-Trioxabicyclo[2.2.2]octane, 1,4-diethyl- | HCID 77843 | — |
Reaction Steps
Into a flask as specified in Example 1 were charged 529 g of triethyl orthopropionate, 402 g of trimethylol propane, 330 g of diethylene glycol dimethyl ether, and 0.9 g of PTSA. The mixture was heated for 0.5 hour at 140° C., with 402 g of ethanol being distilled off. The temperature was lowered to 100° C., and the remaining diethylene glycol dimethyl ether was distilled off under reduced pressure. The residue was subjected to vacuum distillation. The fraction having a boiling temperature of 54° C. at a pressure of 0.5 mbar yielded 370 g of clear, low-viscous liquid having a boiling point of 223° C. at atmospheric pressure and with the following structure
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06297329B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-fee2c1939b754f3aa0d880dbf10e2afc |
| Source note | uspto-grants-2001_10 |