참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Neopentyl alcohol | HCID 6404 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 3-(Tert-butoxy)-2,2-dimethyl-3-oxopropanoic acid | HCID 254415 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 2,2-Dimethylmalonic acid t-butyl ester (2,2-dimethylpropyl)ester | HCID 86677399 | — |
반응 단계
To a mixture of 2,2-dimethylmalonic acid mono-t-butyl ester (10 g), 2,2-dimethyl-1-propanol [CAS No. 75-84-3] (5.15 g), DMAP (1.3 g), and dichloromethane (100 mL), WSC (12.2 g) was added with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 2 days. TBME and water were added to the mixture, and the resulting mixture was extracted. The organic layer was sequentially washed with water and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain 2,2-dimethylmalonic acid t-butyl ester(2,2-dimethylpropyl)ester (12 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08436009B2 |
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| 출처 데이터셋 | uspto-grants-2013_05 |
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| ORD ID | ord-9c026640a7af4bcfa1c86a1ce392f220 |
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| 출처 메모 | uspto-grants-2013_05 |
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