関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 2,6-Dimethylphenol | HCID 11335 | — |
| 反応物 | 3-Hydroxy-2,2-dimethylpropionaldehyde | HCID 11699 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(3-Hydroxy-2,2-dimethylpropyl)-2,6-dimethylphenol | HCID 19088213 | 92% |
反応手順
125 g (1 mol) of 80% strength aqueous 2,2-dimethyl-3-hydroxypropanal (crude mixture from the synthesis, reduced to a water content of 20%. by distillation), 109 g (0.9 mol) of 2,6-dimethylphenol, 12 g (0.11 mol) of 40% strength aqueous dimethylamine and 700 g of methanol are reacted in a stirred autoclave at 180° C. under autogenous pressure of 20-30 bar for 10 h. After the autoclave has cooled and the pressure has been released, 19 g of Raney Ni (0.02 parts based on complete mixture) are added to the reaction mixture and hydrogenation is carried out at 80° C. under 80 bar of hydrogen for 5 h. Workup of the mixture by distillation yields 174 g (92%) of 3-(3,5-dimethyl-4-hydroxyphenyl)-2,2-dimethylpropanol (boiling point 172°-174° C.; melting point 133°-134° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05304685 |
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| 出典データセット | uspto-grants-1994_04 |
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| ORD ID | ord-8e392b9e2967487bafd2fb5bc2cdb069 |
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| 出典メモ | uspto-grants-1994_04 |
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