Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Propanol | HCID 1031 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Cyclohexane | HCID 8078 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 12731072 | HCID 12731072 | — |
Reaction Steps
To 841.4 g of n-propanol, 1750 g of cyclohexane, and 6.7 g of p-toluenesulfonic acid placed in a 4 liter three-necked flask fitted with a stirrer, dropping funnel, reflux condenser, and internal thermometer, 602.7 g of 3-methylbutyrladehyde is added with stirring over a period of 5 minutes. Owing to the acetal formation which starts spontaneously, the internal temperature rises to about 35° C. The mixture is allowed to react at 35° C. to 40° C. for 30 minutes, a pH of 7.0 is then established in the reaction mixture, which is composed of a lower water phase and an upper organic phase, by addition of sodium hydroxide solution (20% aqueous solution), and the water phase is separated. To remove the low-boiling components, the organic phase is subjected to initial distillation at 200 mbar and a bottom temperature up to 100° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05354911 |
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| Source dataset | uspto-grants-1994_10 |
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| ORD ID | ord-8fa3db1f66b14b7ebce45ad9dfdf5e9c |
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| Source note | uspto-grants-1994_10 |
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