참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylene Glycol | HCID 174 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | Ethyl levulinate | HCID 10883 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Ethyl 2-methyl-1,3-dioxolane-2-propionate | HCID 70332 | — |
반응 단계
A mixture of about 110.86 g of ethylene glycol, about 2 g of p-toluenesulfonic acid and about 800 ml of toluene was refluxed using a Dean-Stark trap until no more water came off. An about 250 g portion of ethyl levulinate was added and refluxing was continued until no more water came off. The mixture was then cooled to room temperature, poured into saturated sodium bicarbonate, the organic layer dried and the solvent removed. The residue was distilled (about 67°-70° C., 0.35 mm) and the distillate stirred for about 20 minutes with about 6 g of sodium borohydride in ethanol. The solvent was removed, the residue dissolved in ether, washed with saturated sodium bicarbonate, dried and then distilled (about 41°-45° C., 0.3 mm), giving about 83 g of the desired title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04640913 |
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| 출처 데이터셋 | uspto-grants-1987_02 |
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| ORD ID | ord-2ae60c5edcd243dd857201c80ff05cdc |
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| 출처 메모 | uspto-grants-1987_02 |
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