関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-2-butene | HCID 10553 | — |
| 反応物 | 4-(4-Trifluoromethylphenyl)thiophene-2-carbaldehyde | HCID 11736954 | — |
| 反応物 | Sodium Chlorite | HCID 23668197 | — |
| 反応物 | Monosodium phosphate | HCID 23672064 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 4-[4-(Trifluoromethyl)phenyl]thiophene-2-carboxylic acid | HCID 21986512 | — |
反応手順
A solution of 4-[4-(trifluoromethyl)phenyl]thiophene-2-carbaldehyde (intermediate 37, 1.23 g), t-butanol (20 ml) and 2-methyl-2-butene (10 ml) was cooled to 0° C. To this was added drop-wise, a solution of sodium chlorite (3.8 g) and sodium dihydrogen phosphate (4.03 g) in water (15 ml). After the addition was complete, the mixture was allowed to warm to room temperature and was stirred for 4 hours. The solution was then concentrated and partitioned between water and ethyl acetate. The aqueous layer was washed with a second ethyl acetate portion and the organic liquors were combined, washed with brine, then dried (MgSO4). The solution was then absorbed onto silica and loaded onto a SPE (Si) cartridge. The product was eluted with neat ethyl acetate to afford the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091237B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-6f39bd3263d74268b672227e11e8ee23 |
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| 出典メモ | uspto-grants-2006_08 |
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