참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | HCID 13349246 | HCID 13349246 | — |
| 반응물 | Diethyl aluminum chloride | HCID 16686102 | — |
| 촉매 | Phosphoric Acid | HCID 1004 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 13349252 | HCID 13349252 | 90% |
반응 단계
After 0.63 ml (0.63 mmol) of diethylaluminum chloride (hexane 1M solution) were added to a dried methylene chloride (3 ml) solution of 89.7 mg (0.24 mmol) of (S)-2-methanesulfonyloxy-3-octyl-3-undecanol (unrefined) at -78° C. under stirring, and stirred for two and a half hours at -78° C., the temperature was raised to 0° C. over an hour and a half. The reaction was stopped with three drops of phosphoric acid buffer solution (pH 7). The resultant suspension was diluted with ethyl acetate, dried with anhydrous sodium sulfate, filtered and concentrated. The oily residue was separated and refined by the use of silica gel column chromatography (hexane/ethyl acetate=35/1) to obtain (S)-10-methyl-9-octadecanone as a colorless oily substance (60.5 mg, yield 90%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04604486 |
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| 출처 데이터셋 | uspto-grants-1986_08 |
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| ORD ID | ord-524551429d3e4fc2bae4047df7efb279 |
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| 출처 메모 | uspto-grants-1986_08 |
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