Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | 4-Fluoro-3-(trifluoromethyl)benzaldehyde | HCID 522269 | — |
| Edukt | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Edukt | (R)-1-(3-fluoro-5-(trifluoromethyl)phenyl)-1-(4-fluorophenyl)-2-phenylethanamine | HCID 59458936 | — |
| Lösungsmittel | 1,1-Dichloroethane | HCID 6365 | — |
| Produkt | HCID 23582336 | HCID 23582336 | 55,5% |
Reaktionsschritte
(R)-1-(3-fluoro-5-(trifluoromethyl)phenyl)-1-(4-fluorophenyl)-2-phenylethanamine (21.5 mg, 0.057 mmol) in dichloroethane (0.5 mL) in a two drum vial was added 4-fluoro-3-(trifluoromethyl)benzaldehyde (21.9 mg, 0.114 mmol) followed by a drop of acetic acid. The reaction mixture was shaken for 20 minutes at room temperature before NaBH(OAc)3 (36.3 mg, 0.171 mmol) was added. The reaction was stirred at room temperature overnight. The solvents were removed and the residue was purified by preparative HPLC (phenominex C18 column, 21×100 mm, 5μ) using MeOH/H2O (with 0.1% TFA) to give (R)—N-(4-fluoro-3-(trifluoromethyl)benzyl)-1-(3-fluoro-5-(trifluoromethyl)phenyl)-1-(4-fluorophenyl)-2-phenylethanamine as a colorless oil (17.5 mg, 46% yield). LCMS: 4.32 min (4 min gradient, MeOH/H2O 0.1% TFA); 1H NMR (400 MHz, CDCl3) δ ppm 3.78-3.91 (m, 4H), 6.60 (d, J=7.47 Hz, 2H), 7.14-7.27 (m, 7H), 7.35-7.48 (m, 6H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08642576B2 |
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| Quelldatensatz | uspto-grants-2014_02 |
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| ORD ID | ord-68f95fc6c830425bb321c07937e0e57f |
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| Quellennotiz | uspto-grants-2014_02 |
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