化工社化工社 化学情報印刷レポート · 研究参考用
Benzaldehyde dimethyl acetal → 5-Methyl-2-phenyl-1,3-dioxane-5-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzaldehyde dimethyl acetal | HCID 62375 | — |
| 反応物 | Dimethylolpropionic acid | HCID 78501 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-Methyl-2-phenyl-1,3-dioxane-5-carboxylic acid | HCID 704798 | — |
反応手順
Into a round bottom flask was added sequentially 3-hydroxy-2-hydroxymethyl-2-methyl-propionic acid (10.0 g, 74.5 mmol), acetone (75.0 mL), benzaldehyde dimethyl acetal (17.02 g, 111.0 mmol) and para-toluenesulfonic acid monohydrate (0.71 g, 3.7 mmol). The resulting mixture was stirred at ambient temperature for 4 h and then filtered. The filter cake was rinsed with cold acetone and dried under vacuum to give the title compound as a white solid. 1H NMR (CDCl3, 300 MHz) δ (ppm): 7.46-7.48 (m, 2H), 7.34-7.36 (m, 3H), 5.49 (s, 1H), 4.65 (d, J=10.8 Hz, 2H), 3.70 (d, J=11.4 Hz, 2H), 1.11 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08927573B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-a253150411e1445f99e2876e2e371706 |
| 出典メモ | uspto-grants-2015_01 |