HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Trimethylolpropane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl- | HCID 11816152 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Trimethylolpropane | HCID 6510 | 179.7% |
Reaction Steps
7.8 g (17 mmol) of the crude sulfonate 6 prepared in step 2 are introduced into 60 ml of methanol, and 3 N hydrochloric acid is added dropwise until the pH is less than 5. 400 mg of p-toluenesulfonic acid are subsequently added, the mixture is stirred at room temperature for 21 hours, and methanolic potassium hydroxide solution is added until the mixture is slightly alkaline (pH≈8 to 9). The solvent is removed by distillation in vacuo, and the residue which remains is separated by column chromatography on silica gel using dichloromethane as the eluent, giving 4.1 g of a colorless oil 7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05191069 |
| Source dataset | uspto-grants-1993_03 |
| ORD ID | ord-93887c0091264eff95cab08348e34c0f |
| Source note | uspto-grants-1993_03 |