참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 4,4,4,4',4',4'-Hexafluorovaline | HCID 85954 | — |
| 반응물 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3,3,3-Trifluoro-2-(trifluoromethyl)-1-(hydroxymethyl)propylamine | HCID 45107971 | — |
반응 단계
A solution of 4,4,4,4′,4′,4′-hexafluoro-DL-valine (0.500 g, 2.22 mmol) in THF (20 mL) was stirred under nitrogen at 25° C. Borane-THF complex (6.66 mL, 1.0 M in THF) was added dropwise and the resulting solution stirred for 4 h at 25° C. After this time period, the reaction was complete by TLC (10:2:1 EtOAc:EtOH:H2O). The reaction mixture was quenched by slow addition of 10% HOAc in MeOH (23 mL). After concentration, the residue was dissolved in Et2O (200 mL) and washed with saturated aqueous NaHCO3 (3×20 mL) and brine (20 mL), and then dried using Na2SO4. After concentration, the resulting residue was used directly in the next reaction without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07547725B2 |
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| 출처 데이터셋 | uspto-grants-2009_06 |
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| ORD ID | ord-572a1b43fd71487f8387137449386527 |
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| 출처 메모 | uspto-grants-2009_06 |
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