関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyclohexanone | HCID 7967 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,1-Dibutoxycyclohexane | HCID 243718 | 187.7% |
反応手順
In a 300-ml three-necked flask equipped with a water separator, 98 g (1 mole) of cyclohexanone, 148 g (2 moles) of n-butanol, 2.4 mg of stannous chloride dihydrate and 40 g of toluene were charged. The resulting mixture was heated at 125° C. under atmospheric pressure for 6 hours in a nitrogen atmosphere while removing the water formed from the reaction mixture by azeotropic distillation. When water was no longer distilled, the solvent (toluene) and unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 214.3 g of cyclohexanone dibutyl acetal [R1, R2 =a pentamethylene group and R3 =a n-butyl group] (boiling point: 102° C./3 mmHg) (yield: 94.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05792876 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-542f35a4804e41f38e9363201eecef33 |
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| 出典メモ | uspto-grants-1998_08 |
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