関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroquinone | HCID 785 | — |
| 反応物 | Methyl Methacrylate | HCID 6658 | — |
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | 1-Decanol | HCID 8174 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 触媒 | zinc;(Z)-4-oxopent-2-en-2-olate | HCID 5360437 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Decyl methacrylate | HCID 18510 | 99.1% |
反応手順
To a 1 liter flask equipped with an agitator, thermometer and a Vigreux fractionating column were added 188 g (1.88 mol) of methyl methacrylate (MMA), 59.4 g (0.376 mol) of n-decyl alcohol, 1.25 mol % of zinc acetylacetonate, 1.25 mol % of LiCl and 0.75 g of phenothiazine, and 0.62 g of hydroquinone free radical polymerization inhibitor. The mixture was heated to reflux at atmospheric pressure while an azeotropic mixture of MMA and methanol was removed from the upper part of the fractionation column. The reaction was continued in this manner for approximately five hours. After vacuum filtration of the catalyst and inhibitors, the excess of MMA was removed under vacuum and the resulting n-decyl methacrylate (DMA) was isolated (84.3 grams, 99.1% yield) and analyzed. Gas-liquid chromatographic (GLC) analysis showed 99% conversion of 1-decanol to DMA of 98% purity.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08865931B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-9b6b581d4a754dddad895a3cb06d7e05 |
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| 出典メモ | uspto-grants-2014_10 |
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