関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Isobutyraldehyde | HCID 6561 | — |
| 反応物 | m-Xylyl chloride | HCID 12102 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzenepropanal, alpha,alpha,3-trimethyl- | HCID 13797308 | — |
反応手順
A pre-mix of 23.3 g of NaOH, 2.5 g of tetrabutylammonium iodide, 107 ml of water, 25 ml of toluene and 9 ml of tetrahydrofuran under argon was heated to 70° C. A mixture of 70 g (0.5 moles) of 3-methylbenzyl chloride and 50.4 g (0.7 moles) of isobutyraldehyde was added dropwise to this pre-mix within a period of 2 hours while stirring vigorously. The reaction mixture was then maintained at a temperature of 75° C. for 3 hours. After separating the phases and removing the solvents, 66.5 g of end product were obtained by fractional distillation at 0.12 mbar in a temperature range of from 50° C. to 52° C.
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-fc35e75704424c6e9b73e486389cf5f4 |
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| 出典メモ | uspto-grants-1987_12 |
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