関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Dimethylolpropionic acid | HCID 78501 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 5-Methyl-2-phenyl-1,3-dioxane-5-carboxylic acid | HCID 704798 | 81.8% |
反応手順
435 g of benzaldehyde and 550 g 2,2-bis(hydroxymethyl)propanoic acid were allowed to react in the presence of a small amount of p-toluenesulphonic acid. The reaction was under stirring carried out at room temperature followed by heating to 40° C. under a low pressure (15 mm Hg). Yielded product was then dissolved in a mixture of 8000 ml aqueous sodium hydrogencarbonate (0.54M) and 2500 ml of diethyl ether. The aqueous phase was now washed with diethyl ether and acidified with 800 g of tartaric acid. The precipitate was collected and washed with water. Obtained product was finally recrystallized from ethanol/ethyl acetate to yield 745 g of 5-methyl-2-phenyl-1,3-dioxane-5-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211329B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-08c934b3ad7b41c78e673c74fd854371 |
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| 出典メモ | uspto-grants-2001_04 |
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