참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Magnesium perchlorate | HCID 24840 | — |
| 반응물 | HCID 178472487 | HCID 178472487 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178472492 | HCID 178472492 | — |
| 생성물 | HCID 178472493 | HCID 178472493 | — |
반응 단계
To a solution of cis/trans-4-hydroxycyclohexane carboxylic acid ethyl ester (2:1) (1.0 g, 5.8 mmol) and di-tort-butyl dicarbonate (2.9 g, 13.4 mmol) in dichloromethane (6 ml) was added anhydrous magnesium perchlorate (0.13 g, 0.58 mmol) which was previously activated in high vacuo (ca. 1 mbar) at 150° C. for 1 h. Stirring for 16 h at 40° C. was followed by partitioning between dichloromethane (50 ml) and water (30 ml). The layers were separated. The aqueous layer was extracted with one 50-ml portion of dichloromethane. The combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo. Purification by flash-chromatography with n-heptane/tert-butyl methyl ether as eluent gave pure trans-4-tert-butoxy-cyclohexanecarboxylic acid ethyl ester and cis-4-tert-butoxy-cyclohexanecarboxylic acid ethyl ester.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642590B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-ff3942f6ef564a28963eefe7a0353ea6 |
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| 출처 메모 | uspto-grants-2014_02 |
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