関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 反応物 | Dibutylphosphite | HCID 23414612 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 触媒 | Magnesium Chloride | HCID 5360315 | — |
| 生成物 | Dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate | HCID 86241711 | 92.3% |
反応手順
Into a two-liter four-necked flask provided with a stirrer, a thermometer, dropping device, a hydrochloric-acid-recovering device and a condenser, 213.4 g (1.1 moles) of dibutylphosphite, 5.6 g (0.06 moles) of triethylamine and 1.05 g (0.011 moles) of magnesium chloride were fed. While stirring the resulting mixed solution at 25° C., 120.0 g (1.2 moles) of methyl isobutyl ketone (MIBK) was added thereto in 1 hour. The resulting mixed solution was further stirred for 1 hour at the same temperature (25° C.) to complete the reaction. Thereafter, the mixed solution was washed to remove the low-boiling point portions, as in (synthesis of raw material 2) of Example 1, and thus, the triethylamine and the magnesium chloride was removed from the mixed solution, to obtain 298.8 g of dibutyl(1-hydroxy-1,3-dimethylbutyl)phosphonate (raw material 3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728162B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-c4dbe71e53fe47f5aca8f35e02e13474 |
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| 出典メモ | uspto-grants-2010_06 |
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