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CAS No. : | 1035689-60-1 | MDL No. : | |
Formula : | C14H14FNO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 231.27 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | With potassium carbonate;tetrakis(triphenylphosphine) palladium(0); In methanol; toluene; at 80℃; | INTERMEDIATE 1 3'-Ethoxy-3-fluorobiphenyl-4-amine; To a solution of 4-bromo-2-fluoroaniline (3.2g, 17.05mmol), 2M K2CO3 (24ml, 48.00mmol), Pd(PPh3J4 (1.2g, 1.02mmol) in toluene (120ml) under nitrogen atmosphere was added dropwise a solution of the <strong>[90555-66-1]3-ethoxyphenylboronic acid</strong> (4.25g, 25.61 mmol) in 31 ml of MeOH. The mixture was heated to 8O0C overnight and then cooled to room temperature. Ethyl acetate was added and washed twice with a K2CO3 aqueous solution. The organic layer was washed with brine, dried over magnesium sulphate, filtered and the solvent evaporated under vacuum. The residue obtained was purified by flash chromatography eluting with Hexane/ AcOEt (from 10/1 to 8/1). The solid obtained was recrystallized in hexane to yield 3.78 g of the desired compound as a white solid. Yield=72% LRMS: m/z 232 (M+1 )+. Retention time: 6.44 min1 H NMR (250 MHz, CDCI3) delta ppm: 1.4 (t, J=6.9 Hz, 3H); 4.1 (q, J=6.9 Hz, 2H); 6.8 (m, 2H); 7.1 (m, 2H); 7.2-7.3 (m, 3H). |
0.73 g | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In ethanol; water; toluene;Inert atmosphere; Reflux; | Toluene (9 mL), ethanol (6 mL) and water (3 mL) were added into the mixture of M3(0.95 g, 5 mmoi), 3Methoxyhoronic acid (0.83 g, 5 mmoi) and potassium carbonate(1.73 g, 12.5 mn:ioi), stirred with nitrogen replacement for three times. Additionalreplacement with nitrogen was performed for three times after 0.3 g of tetraphenylphenylphosphine palladium was added, Then the reaction was warmed up for refiux reaction ovemght. The product was filtered and concentrated, then 20 mL of dichioromethane and 10 mL of water were added and stirred for 10 mm. The liquid wasseparated and washed with 1 0 mL of water twice, dried with anhydrous sodium sulfate, filtered, concentrated and purified by column chromatography. With 0.73 g of M5 achieved. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | With caesium carbonate;tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 120℃; | INTERMEDIATE 22Methyl 3-(3'-ethoxy-3-fluorobiphenyl-4-ylamino)isonicotinate; A mixture of <strong>[98273-79-1]methyl 3-chloroisonicotinate</strong> (1.00 g, 5.83 mmol), intermediate 1 (1.35 g, 5.83 mmol), Cs2CO3(2.66 g, 8.16 mmol) and Xantphos (0.68 g, 1.17 mmol) in dioxane (20 mL) was stirred under argon atmosphere for 10 min. Then Pd2(dba)3 (0.53 g, 0.58 mmol) was added and the mixture stirred under argon atmosphere at 12O0C overnight. The reaction mixture was filtered over Celite and washed with CH2CI2. The filtrate was concentrated and purified by column chromatography eluting with EtOAc/hexane/Et3N (20/79/1) and the desired compound was obtained. Yield=51% LRMS: m/z 367 (M+1 )+.1H NMR (250 MHz1 CDCI3) delta ppm: 9.26 (s, 1 H); 8.8 (s, 1H); 8.25 (d, J = 5.3 Hz, 1 H); 7.87 (d, J = 5.3 Hz, 1 H); 7.72-7.45 (m, 4H); 7.3 (d, J = 8.2 Hz, 1 H); 7.26 (s, 1H); 7.05 (dd, J = 8.2, J= 1.8 Hz, 1 H); 4.25 (c, J = 7 Hz, 2H); 4.12 (s, 3H); 1.61 (t, J = 7 Hz, 3H). |