Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Product | HCID 13778953 | HCID 13778953 | — |
Reaction Steps
A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (190 g), ethylene glycol (155 g), p-toluenesulfonic acid (2 g) and toluene (200 mL). The reaction mass was heated to reflux (110-130° C.). Water (27 mL) was collected in the Dean Stark trap. When no water was recovered, the reaction mass was cooled to an ambient temperature, neutralized with 10% aqueous sodium carbonate (100 mL) and washed with brine. Purification by vacuum distillation afforded 6,10-dimethyl-1,4-dioxaspiro[4,5]decane (225 g), which had a boiling point of 93° C. at a pressure of 22 mmHg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07547667B1 |
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| Source dataset | uspto-grants-2009_06 |
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| ORD ID | ord-6567baefffb44eb58088bc0e7d7bc0d2 |
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| Source note | uspto-grants-2009_06 |
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