関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Cyclohexanone | HCID 7967 | — |
| 反応物 | Propane, 2,2',2''-[methylidynetris(oxy)]tris- | HCID 78191 | — |
| 触媒 | Iron chloride (FeCl3) | HCID 24380 | — |
| 生成物 | 1-Isopropoxycyclohexene | HCID 4366136 | 92% |
反応手順
A mixture of 190.3 g (1 mol) triisopropyl orthoformate, 98.15 g (1 mol) of cyclohexanone and 6.00 g (0.10 mol) of isopropanol was placed in a three-neck round bottom flask and cooled to about 5° C. in an ice bath. The mixture was stirred and 0.4 g (2 mmol) of reagent grade iron (III) chloride was added. Upon addition of the FeCl3 catalyst, the temperature of the mixture rose to about 15-20° C., indicating that the reaction was proceeding. The mixture was stirred at 20° C. until gas-chromatographic (“GC”) analysis indicated completion of the reaction. The by-products isopropyl formate and isopropanol were removed by distillation under reduced pressure. The remaining residue was subsequently distilled to provide 1-isopropoxy-1-cyclohexene (bp 34° C. @3 mm Hg) as a colorless liquid; the yield was 92% with a purity exceeding 99%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06235944B1 |
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| 出典データセット | uspto-grants-2001_05 |
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| ORD ID | ord-8fe0e5a4ca284a75be776bb6640a2d22 |
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| 出典メモ | uspto-grants-2001_05 |
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