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 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Methyl Benzoin | HCID 98097 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydroxy-2-methoxy-1,2-diphenylpropan-1-one | HCID 21909513 | — |
反応手順
Potassium hydroxide 0.4 g was dissolved in ethanol 5 mL and dimethyl sulfoxide 200 mL was further added to obtain a solution. Benzoin methyl ether 30 g (0.13 mol) was dissolved in the solution and paraformaldehyde 5 g (0.16 mol) was added and reacted at 40° C. for 3 hours under nitrogen current. After that, the reaction product was cooled to a room temperature and neutralized with a dilute hydrochloric acid and then saturated salt water 120 mL was added. The solution was extracted by ethyl acetate and the extracted liquid was washed with saturated salt water three times. The washed product was dried and concentrated by anhydrous magnesium sulfate and recrystallized by diethyl ether. α-methylol benzoin methyl ether (MBME) was obtained in such a manner.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07253131B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-7a309612a73f478487bc80aaed6533eb |
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| 出典メモ | uspto-grants-2007_08 |
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