関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Hydroxyisophthalaldehyde | HCID 165106 | — |
| 反応物 | 2-Bromomethyl-4-tert-butylthiazole | HCID 19603750 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Tert-butyl-2-(2,4-diformylphenoxymethyl)thiazole | HCID 19092782 | 73.5% |
反応手順
A mixture of 2-bromomethyl-4-tert-butylthiazole (1.05 g), 5-formyl-2-hydroxybenzaldehyde (0.74 g), potassium carbonate (0.89 g) and potassium iodide (small mass) in N,N-dimethylformamide was stirred at 50° C. for 5 hours. After being cooled, the resulting solution was poured into ice-water and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated under reduced pressure to give a syrup. The syrup was subjected to column chromatography on silica gel and eluted with a mixture of toluene and ethyl acetate. The fractions containing object compound were combined and concentrated under reduced pressure to give 4-tert-butyl-2-(2,4-diformylphenoxymethyl)thiazole (1.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05296495 |
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| 出典データセット | uspto-grants-1994_03 |
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| ORD ID | ord-5a3bfa456f6442678f9e09506ade3b88 |
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| 出典メモ | uspto-grants-1994_03 |
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