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HRID 477426作成日:2026年10月27日

Sodium Carbonate → Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-

https://huagongshe.com/reaction/477426

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物2,4-DI-Tert-butylcyclohexanolHCID 546032—
反応物Jones' reagentHCID 131709961—
溶媒AcetoneHCID 180—
溶媒IsopropanolHCID 3776—
生成物Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-HCID 114442100.2%

反応条件

温度5 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US04888323
出典データセットuspto-grants-1989_12
ORD IDord-eea22d50aed44f19ac315f7d527947c8
出典メモuspto-grants-1989_12