関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Methyl-2-phenyl-thiazole-5-carboxylic acid | HCID 720957 | — |
| 反応物 | 6,6-Difluoro-5-methyl-5-hexenyl methanesulfonate | HCID 23020371 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6,6-Difluoro-5-methyl-5-hexenyl 4-methyl-2-phenylthiazole-5-carboxylate | HCID 23020188 | 74% |
反応手順
To 10 ml of N,N-dimethylformamide were dissolved 0.50 g (2.2 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 0.53 g (2.4 mmol) of 4-methyl-2-phenylthiazole-5-carboxylic acid, followed by the addition of 0.37 g (4.4 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 6 hours. The reaction liquid was then poured in water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:19) to obtain 0.57 g (yield: 74%) of 6,6-difluoro-5-methyl-5-hexenyl 4-methyl-2-phenylthiazole-5-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07273878B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-ed3a289d1c7047d889f544ad0741d157 |
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| 出典メモ | uspto-grants-2007_09 |
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