関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl chloride | HCID 7850 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Methyl-2-(2-methylphenyl)butanenitrile | HCID 14245130 | — |
| 触媒 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | alpha-Allyl-alpha-isopropyl-2-methylbenzyl cyanide | HCID 19933531 | 93% |
反応手順
To a solution of 362 g of sodium hydroxide in 362 ml of demineralized water 216.6 g of α-isopropyl-2-methylbenzyl cyanide and 6.4 g of tetrabutylammonium hydrogen sulfate were added, and the mixture was heated to 40° C. with intensive stirring. During 3hours 287 g of allylchloride was added. During, the addition and for further two hours the temperature of the reaction mixture was maintained at 40° C. and thereafter at 60° C. for additional three hours. After cooling to room temperature, the reaction mixture was diluted with 550 ml of water and the product was extracted into toluene. After washing with water until neutral pH and drying with anhydrous magnesium sulfate, the solvent was evaporated and the residue was distilled under diminished pressure to obtain 249 g (93%) of the desired compound, b.p. 122°-124 ° C./333 Pa.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424456 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-4885e1af76354a0da3de3354ae290034 |
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| 出典メモ | uspto-grants-1995_06 |
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