関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Ethyl-2-hydroxybenzaldehyde | HCID 10236017 | — |
| 反応物 | 4-Methylsulfonyloxymethyl-1,3-dioxane | HCID 18941616 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Ethyl-2-(1,3-dioxan-4-ylmethoxy)benzaldehyde | HCID 18941614 | 55.3% |
反応手順
A stirred solution of 3.8 grams (0.026 mole) of 5-ethyl-2-formylphenol, 5.0 grams (0.026 mole) of 4-methylsulfonyloxymethyl-1,3-dioxane, and 7.0 grams (0.051 mole) of potassium carbonate in 150 mL of N,N-dimethylformamide was heated at 80° C. for about 18 hours. Analysis by thin layer chromatography (TLC) indicated the reaction was not complete. An additional 2.5 grams (0.013 mole) of 4-methylsulfonyloxymethyl-1,3-dioxane was added, and the reaction mixture was heated at 80° C. for an additional five hours. After this time the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with aqueous 10% lithium chloride, dried with magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure to a residue. The residue was purified by column chromatography on silica gel, yielding 3.6 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | USH0001759 |
|---|
| 出典データセット | uspto-grants-1998_11 |
|---|
| ORD ID | ord-78ee1c41d0214d01899771ef4a24d8d5 |
|---|
| 出典メモ | uspto-grants-1998_11 |
|---|