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Neopentyl glycol → 2-((Benzyloxy)methyl)-5,5-dimethyl-1,3-dioxane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 反応物 | (Phenylmethoxy)acetaldehyde | HCID 108989 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-((Benzyloxy)methyl)-5,5-dimethyl-1,3-dioxane | HCID 59792557 | 96.6% |
反応手順
To a mixture of benzyloxyacetaldehyde (5 g, 33.3 mmol), 2,2-dimethyl-1,3-propanediol (4.16 g, 40 mmol) and toluene (70 ml), p-toluenesulfonic acid monohydrate (287 mg, 1.51 mmol) was added and refluxed for 4 hours while removing water by the Dean-Stark apparatus. After the reaction mixture was cooled to room temperature, triethylamine (4 ml) was added to the reaction mixture and the solvent was removed by evaporation. The residue was purified by silica gel column chromatography (silica gel: 200 g, elution solvent: ethyl acetate/heptane=1/9) to obtain the title compound (7.6 g, yield: 96.6%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425634B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-95876f928d594ffb87130057875b8aae |
| 出典メモ | uspto-grants-2008_09 |