참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 3-[(2-Hydroxyethyl)amino]propane-1,2-diol | HCID 15034945 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 2-[(2,2-Dimethyl-[1,3]dioxolan-4-yl-methyl)-amino]-ethanol | HCID 20553666 | 100% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202511B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
|---|
| ORD ID | ord-6da2b1d584e144829554e1d362a652c5 |
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| 출처 메모 | uspto-grants-2012_06 |
|---|