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 | 4,4-Difluoro-3-Methyl-3-Buten-1-Yl Methanesulfonate | HCID 23020237 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,4-Difluoro-3-methyl-3-butenyl 4-methyl-2-phenylthiazole-5-carboxylate | HCID 69178921 | 94% |
反応手順
To 25 ml of N,N-dimethylformamide were dissolved 2.60 g (13 mmol) of 4,4-difluoro-3-methyl-3-butenyl methanesulfonate and 2.19 g (10 mmol) of 4-methyl-2-phenylthiazole-5-carboxylic acid, followed by the addition of 1.68 g (20 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 3 hours. The reaction liquid was then poured in water and extracted with diethyl ether. 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 ether: hexane=1:9) to obtain 3.03 g (yield: 94%) of 4,4-difluoro-3-methyl-3-butenyl 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-c74a8cac6b1e46f7bf1fc4135f11063b |
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| 出典メモ | uspto-grants-2007_09 |
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