関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitro-4-(trifluoromethyl)phenol | HCID 9816 | — |
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | 2-Bromo-2-methylpropanal | HCID 578377 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2-Nitro-4-trifluoromethylphenoxy)isobutyraldehyde | HCID 10683913 | 33.1% |
反応手順
To a mixture of 10 g of 2-nitro-4-trifluoromethylphenol, 8.0 g of anhydrous calcium carbonate and 30 ml of N,N-dimethylformamide was added dropwise a solution of 8.8 g of 2-bromoisobutyraldehyde in 23 ml of N,N-dimethylformamide and the mixture was stirred at room temperature for 4 days. The reaction mixture was then poured in ice-water and extracted with toluene. The organic layer was washed with 0.5 N aqueous sodium hydroxide solution and water in that order and dried over anhydrous magnesium sulfate and the solvent was distilled off. The residue was chromatographed on a silica gel column and elution was carried out with hexane-ethyl acetate (3:1). The Crystals from the eluate were recrystallized from 15 ml of hexane twice to give 4.428 g of 2-(2-nitro-4-trifluoromethylphenoxy)isobutyraldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420126 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-90fe87addf29438a8e3aa7aa6b4f105f |
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| 出典メモ | uspto-grants-1995_05 |
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