関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isobutyraldehyde | HCID 6561 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3,5-Dimethylbenzyl chloride | HCID 137700 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 触媒 | Tetradecyltrimethylammonium bromide | HCID 14250 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,2-Dimethyl-3-(3,5-dimethylphenyl)-propionaldehyde | HCID 13797311 | 92% |
反応手順
A pre-mix of 125 g of 30% by weight sodium hydroxide solution, 5 g of potassium iodide, 10 g of tetradecyltrimethylammonium bromide, 200 ml of tetrahydrofuran and 200 ml of toluene was heated to 75° C. A mixture of 155 g of 3,5-dimethylbenzyl chloride, 110 g of isobutyraldehyde, 50 ml of tetrahydrofuran and 50 ml of toluene was added dropwise to this pre-mix while stirring vigorously. The entire mixture was then boiled under reflux for 6 hours. The phases were then separated and the organic phase was first washed with warm water and then filtered with the addition of activated carbon. Finally, distillation was carried out using a packed column with wire spirals. The distillation, carried out in a temperature range of from 72° C. to 74° C. at 0.25 mbar, yielded 106 g of 92% 2,2-dimethyl-3-(3,5-dimethylphenyl)-propionaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04710316 |
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| 出典データセット | uspto-grants-1987_12 |
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| ORD ID | ord-f2ef4a85e9a04737bae7c8b6c5b234f1 |
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| 出典メモ | uspto-grants-1987_12 |
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