Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 2-(1,1,2,2-Tetrafluoroethoxy)benzaldehyde | HCID 2778814 | — |
| Reactant | HCID 57507187 | HCID 57507187 | — |
| Solvent | Cyclohexane ethylacetate | HCID 21867204 | — |
| Product | HCID 74408212 | HCID 74408212 | 68% |
Reaction Steps
A 10 mL flask was charged with (4-hydrazino-6-morpholin-4-yl-1,3,5-triazin-2-yl)-(4-trifluoromethoxyphenyl)amine (XV) (159 mg, 0.43 mmol), 4-(1,1,2,2-tetrafluoroethoxybenzaldehyde (142 μL, 0.86 mmol), and ethanol (5 mL) and the mixture was stirred at ambient temperature for 24 h. Water (5 mL) was added to the reaction mixture which was then extracted with EtOAc (3×5 mL). The combined organic extract was washed with brine (10 mL), dried over sodium sulfate, filtered, and concentrated under vacuum. Flash chromatography (silica gel, 10% EtOAc/cyclohexane) afforded compound 1 (167 mg, 68% yield): m.p. 203-206° C.; 1H NMR (CDCl3) δ 8.65 (s, 1H), 7.79 (s, 1H), 7.66-7.55 (m, 4H), 7.20-7.12 (m, 4H), 6.10-5.73 (tt, J1=53.1 Hz, J2=2.56 Hz, 1H), 3.86-3.75 (m, 8H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08067588B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-038d182fe7bc4401909d88a38e454dd8 |
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| Source note | uspto-grants-2011_11 |
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