참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2,4-Difluoroacetophenone | HCID 67770 | — |
| 반응물 | HCID 178418630 | HCID 178418630 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-Cyclopropyl-1-(2,4-difluorophenyl)ethanol | HCID 24749679 | — |
반응 단계
1.50 g (9.61 mmol) of 2′,4′-difluoroacetophenone were dissolved at 0° C. in 8 ml of diethyl ether, and 38.4 ml (19.21 mmol) of a 0.5N solution of cyclopropylmagnesium bromide in tetrahydrofuran were slowly added dropwise. Stirring at 0° C. for 1 h was followed by warming to RT, and the reaction solution was mixed with water and ethyl acetate, and the phases were separated. The organic phase was washed with saturated aqueous sodium chloride solution and dried over sodium sulfate, and the solvents were removed in vacuo. The crude product was purified by preparative HPLC (mobile phase: acetonitrile-water gradient) to result in 0.63 g (33% of theory) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08063234B2 |
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| 출처 데이터셋 | uspto-grants-2011_11 |
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| ORD ID | ord-52d7e875ed7d481392633e4421a1c829 |
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| 출처 메모 | uspto-grants-2011_11 |
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