関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,4-DI-Tert-butylcyclohexanol | HCID 546032 | — |
| 反応物 | Jones' reagent | HCID 131709961 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Cyclohexanone, 2,4-bis(1,1-dimethylethyl)- | HCID 114442 | 100.2% |
反応手順
200 g (0.944 mole) of the 2,4-di-tert-butylcyclohexanol as prepared in Synthetic Example 2 and 2 l of acetone were introduced into a 3 l reactor. Then 320 g of a Jones reagent was added dropwise thereto under ice-cooling at 5° C. over 1.5 hour. After completion of the reaction, isopropyl alcohol was added to the reaction mixture until the brown color of the excessive reagent disappeared. Then the reaction mixture was allowed to stand. After separating the acetone reaction solution, the acetone solution was neutralized with sodium carbonate. Then the solution was filtered and the acetone was distilled off under reduced pressure to give 199 g of crude 2,4 di-tert butylcyclohexanone. This product had a cis/trans ratio of 92/8. It was subjected to precision distillation in a Helipack packing column of a number of theoretical plates of 5 to give 160 g of 2,4 di-tert-butyl cyclohexanone (b.p.: 93.5 to 94° C./3 mm Hg). The cis/trans ratio of this product was 94/6.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04888323 |
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| 出典データセット | uspto-grants-1989_12 |
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| ORD ID | ord-eea22d50aed44f19ac315f7d527947c8 |
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| 出典メモ | uspto-grants-1989_12 |
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