関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | 3-Amino-4-(trifluoromethyl)benzoic acid | HCID 642651 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-4-(trifluoromethyl)benzoic acid | HCID 22337570 | — |
反応手順
5.0 g of 3-amino-4-trifluoromethyl-benzoic acid were dissolved using 50 ml of acetic acid. Then, 50 g of ice and 50 ml of a saturated aqueous HBr-solution were added and a solution of 2.0 g NaNO2 in 10 ml of water was added dropwise at 0° C. The reaction mixture was then stirred at room temperature for 10 minutes. Then, the reaction mixture was added dropwise to a suspension of 7.0 g CuBr and 10.9 g CuBr2 in 100 ml of a half-concentrated aqueous solution of HBr. The resulting mixture was then stirred for 2 h at room temperature, then diluted using 21 of water, stirred for 1 h and finally the precipitate was isolated by filtration. The precipitate was dried in vacuo to yield 5.2 g of the title compound that was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09018383B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-5b18156a578b4db88242592fc18235e3 |
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| 出典メモ | uspto-grants-2015_04 |
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