HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1,3-Dioxepin, 2-(1,1-dimethylethyl)-4,7-dihydro-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Butene-1,4-diol | HCID 8065 | — |
| Reactant | Pivalaldehyde | HCID 12417 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 1,3-Dioxepin, 2-(1,1-dimethylethyl)-4,7-dihydro- | HCID 11062630 | 89.9% |
Reaction Steps
A mixture of 430 g (5 moles) of 2,2-dimethylpropanal, 3 g of p-toluenesulfonic acid and 440 g (5 moles) of but-2-ene-1,4-diol in 1000 ml of toluene was refluxed, and the water of reaction formed was removed in the course of 3 hours (h). The mixture was then left to cool to room temperature, 10 ml of a 25% strength sodium hydroxide solution were added to the solution, the mixture was washed neutral with a little water and the toluene was distilled off under reduced pressure at from 50° to 60° C. The residue obtained was distilled under 0.1 mbar to give 702 g of 2-tert-butyl-4,7-dihydro-1,3-dioxepin of boiling point 80° C./32 mbar.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04761489 |
| Source dataset | uspto-grants-1988_08 |
| ORD ID | ord-d179930b3754451789634e378a8dd266 |
| Source note | uspto-grants-1988_08 |