関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 3-[(2-Hydroxyethyl)amino]propane-1,2-diol | HCID 15034945 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2-[(2,2-Dimethyl-[1,3]dioxolan-4-yl-methyl)-amino]-ethanol | HCID 20553666 | 100% |
反応手順
The N-(hydroxyethyl)-amino-2,3-propanediol (16.5 g, 122 mmol) was treated with a solution of HCl in dioxane (33.5 ml, 134 mmol). To this solution were added 2,2-dimethoxypropane (15.3 g, 147 mmol), DMAC (50 mL), and a catalytic amount of para-toluene sulphonic acid (0.006 mol, 1.16 g). The mixture stirred at room temperature for 24 hours. Triethylamine (1 mL) was then added, and the solvents removed by rotary evaporation. The viscous crude mixture was dissolved into triethylamine (30 mL) and ethyl acetate (500 mL) and stirred at RT for 30 min. The mixture was filtered and the collected solid washed several times with ethyl acetate. The filtrate was then evaporated on a high vacuum rotary evaporator at 40° C. to give a yellow liquid (0.122 mol, 99% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08202511B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-6da2b1d584e144829554e1d362a652c5 |
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| 出典メモ | uspto-grants-2012_06 |
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