関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 4-tert-Butylphenol | HCID 7393 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-(1,1-Dimethylethyl)-2-hydroxy-1,3-benzenedimethanol | HCID 150981 | 99% |
反応手順
200 grams (1.331 moles) of para-t-butylphenol and 400 ml. of water were placed in a 2-liter, 3-neck, round bottom flask fitted with a thermometer, a stirrer and a dropping funnel. The flask was placed in a water bath, the contents stirred and 106.6 grams (1.331 moles) of 50% aq. NaOH added. The temperature of the resulting slurry was adjusted to 30° C. (by cooling) and 227 grams (~2.8 moles) of 37% formalin added. The mixture was heated to 60° C. and stirred at that temperature for 4 hours. It was then cooled to 35° C. and 444 ml. (1.331 moles) of 3 N aq. HCl were added. Enough dilute acetic acid was then added to make the mixture just acid. 100 ml. of chloroform was stirred in and the phases allowed to separate. The chloroform layer, containing essentially all of the product resin, was removed, washed once with water, dried by azeotropic distillation and stripped in vacuo. 276 grams (99% yield) of the title product was obtained as a resinous residue which crystallized on standing; equivalent wt. 220 grams per phenolic --OH (vs 212, theoretical).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04164487 |
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| 出典データセット | uspto-grants-1979_08 |
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| ORD ID | ord-b45f44ace5544db9a485d15461ba854c |
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| 出典メモ | uspto-grants-1979_08 |
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