HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → 2-((Benzyloxy)methyl)-2-methyl-1,3-dioxolane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Ethyl orthoformate | HCID 31214 | — |
| Reactant | 1-(Benzyloxy)propan-2-one | HCID 3691284 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | 2-((Benzyloxy)methyl)-2-methyl-1,3-dioxolane | HCID 59792594 | 90.5% |
Reaction Steps
A mixture of 1-benzyloxy-2-propanone (4.94 g, 30.1 mmol), ethylene glycol (20 ml, 359 mmol), triethyl orthoformate (5 ml, 30.1 mmol), and p-toluenesulfonic acid monohydrate (130 mg, 0.683 mmol) was stirred at room temperature for 61.5 hours. To the reaction mixture, a saturated aqueous sodium hydrogen carbonate solution (20 ml) was added and the mixture was extracted twice with chloroform (50 ml) and the organic layer was dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (NH silica gel, elution solvent: heptane/ethyl acetate=1/0 to 4/1 gradient). Desired fractions were concentrated to obtain the title compound (5.67 g, 90.5% yield) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08124780B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-be08dc1ac0964e0ab2af1a7000be2d3c |
| Source note | uspto-grants-2012_02 |