HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Ethyl (2-propyl-1,3-dioxan-2-yl)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | 1,3-Propanediol | HCID 10442 | — |
| Reactant | Ethyl 3-oxohexanoate | HCID 238498 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Product | Ethyl (2-propyl-1,3-dioxan-2-yl)acetate | HCID 59792385 | 80.5% |
Reaction Steps
A mixture of ethyl 3-oxohexanoate (5 g, 31.6 mmol), 1,3-propanediol (3.61 g, 47.4 mmol), trimethyl orthoformate (5.78 ml, 34.8 mmol), and p-toluenesulfonic acid monohydrate (272 mg, 1.58 mmol) was stirred at room temperature for 22 hours. After completion of the reaction, triethylamine (881 μl, 6.32 mmol) was added to the reaction mixture which was then concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (5.5 g, yield: 80.5%) as a light yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08124780B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-d7dfc88dd4f2486aa12d1969aa2027c1 |
| Source note | uspto-grants-2012_02 |