Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2,3-Butanediol | HCID 262 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Product | HCID 57720059 | HCID 57720059 | — |
Reaction Steps
A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (200 g), 2,3-butanediol (315 g), p-toluenesulfonic acid (2 g) and toluene (300 mL). The reaction mass was heated to reflux (110-130° C.). Water (36 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 2,3,6,10-tetramethyl-1,4-dioxaspiro[4,5]decane (265 g)), which had a boiling point of 104° C. at a pressure of 16 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-23dfa52ab24445c69b979b71f0097541 |
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| Source note | uspto-grants-2009_06 |
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