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2-Methoxypropene → (2,2-Dimethyl-1,3-dioxan-5-yl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methoxypropene | HCID 8300 | — |
| 反応物 | Trimethylolmethane | HCID 78432 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2,2-Dimethyl-1,3-dioxan-5-yl)methanol | HCID 3584869 | 55% |
反応手順
A solution of 2-methoxypropene (1 g) in N,N-dimethylformamide (150 ml) was added to 2-(hydroxymethyl)-1,3-propanediol (500 mg). p-Toluenesulfonic acid (10 mg) was added thereto, and the mixture was stirred at room temperature overnight. The solvent was removed by distillation under the reduced pressure, water was added to the residue, and the mixture was extracted with n-butanol. The n-butanol layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using hexane-acetone to give (2,2-dimethyl[1,3]dioxan-5-yl)-methanol (378 mg, yield 55%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560558B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-286338b454554e4489efeb880c1dd36b |
| 出典メモ | uspto-grants-2009_07 |