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Toluene → 2-Pentyl-4,4,7,7-tetramethyl-4,7-dihydro-1,3-dioxepin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Hexanal | HCID 6184 | — |
| 反応物 | 2,5-Dimethyl-3-hexene-2,5-diol | HCID 349974 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Pentyl-4,4,7,7-tetramethyl-4,7-dihydro-1,3-dioxepin | HCID 21284700 | 70.3% |
反応手順
A mixture of 720 g (5 moles) of 2,5-dimethylhex-3-ene-2,5-diol, 3 g of p-toluenesulfonic acid, 500 g (5 moles) of n-hexanal and 1 l of toluene was refluxed, and the resulting water of reaction (115 ml) was separated off in the course of 5.5 h. The mixture was then left to cool, 10 ml of a 25% strength aqueous sodium hydroxide solution were added, the mixture was washed neutral with a little water and the toluene was removed under reduced pressure at from 50° to 60° C. The residue obtained was distilled under 0.1 mbar to give 796 g of 2-pentyl-4,4,7,7-tetramethyl-4,7-dihydro-1,3-dioxepin of boiling point 75° C./0.1 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04761489 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-204a7f32307348a1bc31f43769c92109 |
| 出典メモ | uspto-grants-1988_08 |