참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 1-(2-trifluoromethyl-phenyl)-ethanone O-methyl-oxime | HCID 54513608 | — |
| 촉매 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (1R)-1-(2-(Trifluoromethyl)phenyl)ethylamine | HCID 2782450 | 17.1% |
반응 단계
Sodium borohydride (1.17 g) is added slowly to a flask containing zirconium tetrachloride (1.8 g) in tetrahydrofuran (27 mL). A solution of 1-(2-trifluoromethyl-phenyl)-ethanone O-methyl-oxime (1.34 g) in tetrahydrofuran (7.7 mL) is added and the resulting solution is stirred at 25° C. for 12 hours. The reaction mixture is then cooled to 0° C. and water (16 mL) is slowly added. Excess ammonium hydroxide is added and the solution is extracted twice with ethyl acetate. The organic portion is washed twice with 1N hydrochloric acid. The aqueous (acid) layer is basified with sodium hydroxide and extracted twice with ethyl acetate. The organic layer is then washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The solvent is removed under reduced pressure to provide the desired product as a yellow oil (0.20 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06271236B1 |
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| 출처 데이터셋 | uspto-grants-2001_08 |
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| ORD ID | ord-3e697578ba174cbc989e02fcea4015bc |
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| 출처 메모 | uspto-grants-2001_08 |
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