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Triethylamine → Ethyl (2-propyl-1,3-dioxan-2-yl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trimethyl orthoformate | HCID 9005 | — |
| 反応物 | 1,3-Propanediol | HCID 10442 | — |
| 反応物 | Ethyl 3-oxohexanoate | HCID 238498 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 生成物 | Ethyl (2-propyl-1,3-dioxan-2-yl)acetate | HCID 59792385 | 80.5% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08124780B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-d7dfc88dd4f2486aa12d1969aa2027c1 |
| 出典メモ | uspto-grants-2012_02 |