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-Chloro-3-ethyl-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 14770682 | — |
| 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-chloro-5-ethyl-2-methyl-2H-pyrazole-3-carboxylate | HCID 69181538 | 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 0.45 g (2.4 mmol) of 4-chloro-5-ethyl-2-methyl-2H-pyrazole-3-carboxylic acid, followed by the addition of 0.37 g (4.4 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 7 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 0.52 g (yield: 74%) of 6,6-difluoro-5-methyl-5-hexenyl 4-chloro-5-ethyl-2-methyl-2H-pyrazole-3-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07273878B2 |
|---|
| 出典データセット | uspto-grants-2007_09 |
|---|
| ORD ID | ord-9bacae5831f746ef887ffa4a56025a9f |
|---|
| 出典メモ | uspto-grants-2007_09 |
|---|