Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Benzaldehyde, 3-(1,1,2,2-tetrafluoroethoxy)- | HCID 118803 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | 3-(3-trifluoromethoxyphenoxy)aniline | HCID 10880118 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | HCID 10281896 | HCID 10281896 | 165.6% |
Reaction Steps
EX-19C) To a solution of 3-(3-trifluoromethoxyphenoxy)aniline (1.0 g, 3.7 mmol) from EX-19B and 3-(1,1,2,2-tetrafluoroethoxy)benzaldehyde (0.83 g, 3.7 mmol) in 18.5 mL of dichloroethane was added sodium triacetoxyborohydride (1.0 g, 4.7 mmol) and glacial acetic acid (0.25 mL, 4.3 mmol). The reaction mixture was stirred at room temperature overnight then quenched with saturated aqueous sodium bicarbonate and extracted with methylene chloride. The organic layer was dried over MgSO4 and concentrated in vacuo to give 1.8 g (100%) of the desired [3-(3-trifluoromethoxy-phenoxy)phenyl][[3-(1,1,2,2-tetrafluoroethoxy)phenyl]methyl]amine product as a yellow oil, which was greater than 90% pure by reverse phase HPLC analysis. HRMS calcd. for C22H16F7NO3: 476.1097 [M+H]+, found: 476.1069. This material was carried on to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07700658B2 |
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| Source dataset | uspto-grants-2010_04 |
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| ORD ID | ord-64b0afb7bb274ddcb07b1512a71706b8 |
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| Source note | uspto-grants-2010_04 |
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