関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 1H-Pyrazole, 3-methyl-5-(trifluoromethyl)- | HCID 139077 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Bromo-3-methyl-5-(trifluoromethyl)pyrazole | HCID 2736430 | 100% |
反応手順
Dissolve 5-methyl-3-(trifluoromethyl)pyrazole (1.00 g, 6.66 mmol) in 60% aqueous acetic acid (13 mL). Add sodium acetate (0.819 g, 9.99 mmol) and cool to 0° C. Add bromine (1.17 g, 7.33 mmol) dropwise over 10 min. Stir at 0° C. for 3 hr, then at room temperature for 18 hr. Add ethyl acetate and saturated aqueous sodium sulfite solution. Separate organics and wash one time with saturated aqueous sodium bicarbonate solution followed by saturated aqueous sodium chloride. Dry (magnesium sulfate), filter and concentrate to give 4-bromo-5-methyl-3-trifluoromethyl-1H-pyrazole (1.50 g, 100%). GC-MS: m/z=229 [M+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08202873B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-33e599f9ee714cb982e2ab2c1ef6a0fd |
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| 出典メモ | uspto-grants-2012_06 |
|---|
