化工社化工社 化学情報印刷レポート · 研究参考用
Trimethylolpropane → 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylolpropane | HCID 6510 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,1-Dimethoxyethane | HCID 10795 | — |
| 触媒 | Diammonium molybdate | HCID 61578 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl- | HCID 11816152 | 95% |
反応手順
Trimethylolpropane (10.0 g; 74.6 mmol), 2,2-dimethoxyethane (9.01 g; 86.5 mmol) and p-toluenesulfonic acid monohydrate (0.369 g; 1.94 mmol) were dissolved in tetrahydrofuran (125 mL). The clear solution was stirred at ambient temperature for 24 h. TLC (stained with ammonium molybdate) confirmed near quantitative conversion of the starting triol. The reaction was neutralised with triethylamine (10 mL) and all volatiles were removed in vacuo. Colourless oily residue was passed through a silicagel column (eluent ethyl acetate/cyclohexane 1:1). The eluent was evaporated to provide (5-ethyl-2,2-dimethyl-1,3-dioxan-5-yl)methanol (12.34 g; 95% yield) as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09296835B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-36b3516933c442f9b5823fb96a670468 |
| 出典メモ | uspto-grants-2016_03 |