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CAS No. : | 1700-02-3 | MDL No. : | MFCD00047340 |
Formula : | C9H5Cl2N3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | AMEVJOWOWQPPJQ-UHFFFAOYSA-N |
M.W : | 226.06 | Pubchem ID : | 15549 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
GHS Pictogram: |
* 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 |
---|---|---|
With hydrogenchloride;aluminium trichloride; In sulfolane; methanol; ligroin; water; | EXAMPLE 62 2,4-Bis(2,4-dihydroxy-5-hexylphenyl)-6-phenyl-s-triazine To a 750 mL sulfonation flask equipped with a mechanical stirrer, condenser, dropping funnel and a nitrogen atmosphere are charged 34.0 g (150 mmol) of 2,4-dichloro-6-phenyl-s-triazine, 44.0 g (330 mmol) of aluminum chloride and 100 mL of ligroin (boiling range 110-140 C). To that suspension, 60 mL of sulfolane are added dropwise with stirring over a 15 minute period with the temperature rising to 50 C. A solution of 62.1 g (320 retool) of 4-hexylresorcinol in 60 mL of sulfolane is then added dropwise over a 15 minute period. The temperature rises to 60 C. and hydrogen chloride is evolved. The reaction mixture is heated to 80 C. for four hours. The lower layer of the two-phase mixture is poured into a solution of 50 mL of concentrated hydrochloric acid in 500 mL of methanol and 300 mL of water. The mixture is stirred at room temperature for 14 hours. The product obtained is suspended in 800 mL of water at 80 C. for 1 hour, is isolated by filtration and resuspended under the same conditions, finally isolated and dried at 85 C. under vacuum. The title compound is obtained as a crude orange product (77.0 g) and melts at 230-238 C. It can be used without further purification. 1 H nmr (DMSO-d6) spectrum is consistent with the desired product. Analysis: Calcd for C33 H39 N3 O4: C, 73.2; H, 7.3; N, 7.8. Found: C, 73.2; H, 7.3; N, 7.6. | |
With hydrogenchloride;aluminium trichloride; In sulfolane; methanol; ligroin; water; | EXAMPLE 62 2,4-Bis(2,4-dihydroxy-5-hexylphenyl)-6-phenyl-s-triazine To a 750 mL sulfonation flask equipped with a mechanical stirrer, condenser, dropping funnel and a nitrogen atmosphere are charged 34.0 g (150 mmol) of 2,4-dichloro-6-phenyl-s-triazine, 44.0 g (330 mmol) of aluminum chloride and 100 mL of ligroin (boiling range 110-140 C.). To that suspension, 60 mL of sulfolane are added dropwise with stirring over a 15 minute period with the temperature rising to 50 C. A solution of 62.1 g (320 mmol) of 4-hexylresorcinol in 60 mL of sulfolane is then added dropwise over a 15 minute period. The temperature rises to 60 C. and hydrogen chloride is evolved. The reaction mixture is heated to 80 C. for four hours. The lower layer of the two-phase mixture is poured into a solution of 50 mL of concentrated hydrochloric acid in 500 mL of methanol and 300 mL of water. The mixture is stirred at room temperature for 14 hours. The product obtained is suspended in 800 mL of water at 80 C. for 1 hour, is isolated by filtration and resuspended under the same conditions, finally isolated and dried at 85 C. under vacuum. The title compound is obtained as a crude orange product (77.0 g) and melts at 230-238 C. It can be used without further purification. 1 H nmr (DMSO-d6) spectrum is consistent with the desired product. Analysis: Calcd for C33 H39 N3 O4: C, 73.2; H, 7.3; N, 7.8. Found: C, 73.2; H, 7.3; N, 7.6. | |
With hydrogenchloride;aluminium trichloride; In sulfolane; methanol; ligroin; water; | Example 62 2,4-Bis(2,4-dihydroxy-5-hexylphenyl)-6-phenyl-s-triazine To a 750 mL sulfonation flask equipped with a mechanical stirrer, condenser, dropping funnel and a nitrogen atmosphere are charged 34.0 g (150 mmol) of 2,4-dichloro-6-phenyl-s-triazine, 44.0 g (330 mmol) of aluminum chloride and 100 mL of ligroin (boiling range 110-140 C.). To that suspension, 60 mL of sulfolane are added dropwise with stirring over a 15 minute period with the temperature rising to 50 C. A solution of 62.1 g (320 mmol) of 4-hexylresorcinol in 60 mL of sulfolane is then added dropwise over a 15 minute period. The temperature rises to 60 C. and hydrogen chloride is evolved. The reaction mixture is heated to 80 C. for four horns. The lower layer of the two-phase mixture is poured into a solution of 50 mL of concentrated hydrochloric acid in 500 mL of methanol and 300 mL of water. The mixture is stirred at room temperature for 14 hours. The product obtained is suspended in 800 mL of water at 80 C. for 1 hour, is isolated by filtration and resuspended under the same conditions, finally isolated and dried at 85 C. under vacuum. The title compound is obtained as a crude orange product (77.0 g) and melts at 230-238 C. It can be used without further purification. 1 H nmr (DMSO-d6) spectrum is consistent with the desired product. Analysis: Calcd for C33 H39 N3 O4: C, 73.2; H, 7.3; N, 7.8. Found: C, 73.2; H, 7.3; N, 7.6. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
57% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; for 16h;Reflux; Inert atmosphere; | triphenylene-2-boronic acid (4.20g, 15.4mmol), 2,4-dichloro-6-phenyl-1,3,5-triazine (3.49g, 15.4mmol), and Pd(PPh3)4 ( 0.89 g,and 0.77 mmol) K2CO3 aqueous solution (23.2 ml of 2M, 46.3mmol) together, it was added to THF (200ml). The reaction mixture was thoroughly degassed and heated to reflux for 16 hours under nitrogen. After cooling to room temperature, the solid was collected by filtration, washed with THF and heptane, 2-chloro-4-phenyl-6- (triphenylene-2- yl) as a pale yellow solid 1,3,5-triazine It was obtained (3.7g, 57%). The product was used without further purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; for 10h;Reflux; Inert atmosphere; | 5.0 g (22.12 mmol) of Intermediate L-1 (2,4-dichloro-6-phenyl-s-triazine), 18.12 g (50.87 mmol) of L-5, 7.64 g (55.30 mmol) of potassium carbonate, 1.28 g (1.11 mmol) of Tetrakis (triphenyl phosphine) palladium (0) (PPh3) 4 was added to 100 mL of tetrahydrofuran and 30 mL of water, and the mixture was heated under reflux for 10 hours under a nitrogen stream. The resulting mixture was added to methanol (500 mL), and the crystallized solid was filtered, dissolved in monochlorobenzene, filtered through silica gel / celite, and an organic solvent was removed in an appropriate amount, followed by recrystallization from methanol to obtain Compound A-2 , 63% yield). The result of elemental analysis of the resulting compound A-2 is as follows. |
63% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 10h;Inert atmosphere; | Synthesis Example 63: Synthesis of Compound A-20 Intermediate I-43 (5.0 g, 22.12 mmol), Intermediate I-42 (18.12 g, 50.87 mmol), potassium carbonate (7.64 g, 55.30 mmol), and tetrakis(triphenyl phosphine) palladium (0) (1.28 g, 1.11 mmol) were added to tetrahydrofuran (THF, 100 mL) and water (30 mL) in a 250 mL flask and then, heated and refluxed under a nitrogen stream for 10 hours. The obtained mixture was added to methanol (500 mL) to crystallize a solid, and the solid was filtered, dissolved in monochlorobenzene, filtered with silica gel/Celite, and then, recrystallized with methanol after removing an appropriate amount of an organic solvent to obtain Compound A-20 (8.5 g, 63%). An elemental analysis of Compound A-20 was as follows. (0384) calcd. C45H31N3: C, 88.06; H, 5.09; N, 6.85. found: C, 88.16; H, 5.23; N, 6.63. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 12h;Inert atmosphere; | Synthesis Example 44: Synthesis of Intermediate I-44 Compound I-42 (50 g, 140 mmol) was dissolved in THF (1 L) under a nitrogen environment, Compound I-43 (31 g, 140 mmol) and tetrakis(triphenylphosphine)palladium (1.6 g, 1.4 mmol) were added thereto, and the mixture was stirred. Potassium carbonate saturated in water (48 g, 350 mmol) was added thereto, and the obtained mixture was heated and refluxed at 80 C. for 12 hours. When the reaction was complete, water was added to the reaction solution, and the mixture was extracted with dichloromethane (DCM) and then, filtered after removing moisture with anhydrous MgSO4 and concentrated under a reduced pressure. This obtained residue was separated and purified through flash column chromatography to obtain Compound I-44 (32 g and 70%). HRMS (70 eV, EI+): m/z calcd for C27H18ClN3: 419.1189. found: 419. Elemental Analysis: C, 77%; H, 4% |
59% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water;Reflux; | 2,4-dichloro-6-phenyl-1,3,5-Triazine 1eq (26.9g) and 1,3,2-Dioxaborolane, 4,4,5,5-tetramethyl-2-[1,1 ':3',1''-terphenyl]-5'-yl- 1.1eq(46.7g) was suspended in 350ml of THF and 170ml of distilled water, and then Pd(PPh3)4 0.05eq(6.8g) and potassium carbonate (K2CO3) 2eq (32.9g) was added and stirred under reflux. When the reaction was completed, the solvent was dried, dissolved in dichloromethane, dried over magnesium sulfate (MgSO4), filtered, and the filtrate was recrystallized from nucleic acid to obtain 29.7 g (Y=59%) of intermediate d-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78.11% | 1) Clean all the glass instruments to be used in the experiment, dry and reserve, and install a mechanical stirring rod.First added to the 250mL three-necked flask of the nitrogen protection device<strong>[84-67-3]4,4'-diamino-2,2'-dimethylbiphenyl</strong> (6.7933 g, 32.0 mmol),Catalyst (1.1437g sodium carbonate, 0.1270g sodium hydroxide)And 10 mL of a mixed organic solvent 1,4-dioxane and toluene (volume ratio of 3:1), and heated to reflux until the solid is dissolved to obtain a mixed solution;2) 2,4-Dichloro-6-phenyl-1,3,5-triazine (0.9000 g, 4.0 mmol)Dissolved in 20 mL of 1,4-dioxane, the solution was added to the reaction flask through a constant pressure dropping funnel, and then fully refluxed for 6 h to obtain a mixed reaction solution;3) The reaction solution was poured into 60 mL of ice water, and after standing for a while, the solution was layered, the upper layer was a clear solution, the lower layer was solid precipitated, and the solid was subjected to column chromatography purification to obtain a volume ratio of ethyl acetate. : V petroleum ether = 1:1 as eluent, 1.7953 g of the target product conjugated diamine monomer was obtained, and the yield was 78.11%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 12h;Inert atmosphere; | <strong>[890042-13-4]4,4,5,5-tetramethyl-2-(triphenylen-2-yl)-1,3,2-dioxaborolane</strong> (50 g, 141 mmol) was dissolved in 0.5 L of tetrahydrofuran (THF) under a nitrogen environment, and 2,4-dichloro-6-phenyl-1,3,5-triazine (47.9 g, 212 mmol) and tetrakis(triphenylphosphine)palladium (1.63 g, 1.41 mmol) were added thereto and then, stirred. Subsequently, potassium carbonate saturated in water (48.7 g, 353 mmol) was added thereto and then, heated and refluxed at 80 C. for 12 hours. When a reaction was complete, after adding water to the reaction solution, the mixture was extracted with dichloromethane (DCM), treated with anhydrous magnesium sulfate to remove moisture, filtered, and concentrated under a reduced pressure. This obtained residue was separated and purified through flash column chromatography to obtain Intermediate I-1 (40.1 g, 68%). (0147) HRMS (70 eV, EI+): m/z calcd for C27H16ClN3: 417.1033, found: 417. (0148) Elemental Analysis: C, 78%; H, 4% |
65% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 8h;Inert atmosphere; | Will be purchased from P&H Tech Co., Ltd. (http://www.phtech.co.kr/)<strong>[890042-13-4]4,4,5,5-tetramethyl-2-(triphenylene-2-yl)-1,3,2-dioxaborolane</strong> (100g, 282mmol) dissolved in 0.1L Tetrahydrofuran (THF) was added under nitrogen and purchased from Tokyo Chemical Industry Co. Ltd. (http://www.tcichemicals.com/)2,4-dichloro-6-phenyl-1,3,5-triazine (95.7g, 423mmol) and tetrakis(triphenylphosphine)palladium (2.72g, 2.86mmol), then stirred. Subsequently, a saturated aqueous solution of potassium carbonate (97.4 g, 705 mmol) was added thereto, and then heated to reflux at 80C for 8 hours. When the reaction was completed, water was added to the reaction solution, and the mixture was extracted with dichloromethane (DCM), treated with anhydrous magnesium sulfate to remove moisture, filtered, and concentrated under reduced pressure. The resulting residue was separated and purified by flash column chromatography to obtain Intermediate I-1 (76.6 g, 65%). |
40.1 g | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 12h; | Dissolve 4,4,5,5-tetramethyl-2-(triphenylene-2-yl)-1,3,2-dioxaborane (50g, 141mmol) in 0.5 of a 1L round bottom flask L tetrahydrofuran (THF), add 2,4-dichloro-6-phenyl-1,3,5-triazine (47.9g, 212mmol) and tetrakis(triphenylphosphine) palladium (1.63g, 1.41 mmol), and the resulting mixture was stirred. Subsequently, a saturated aqueous solution of potassium carbonate (48.7 g, 353 mmol) was added thereto, and the resulting mixture was heated and refluxed at 80C for 12 hours. When the reaction was completed, water was added to the reaction solution, and the resultant was extracted with dichloromethane (DCM), treated with anhydrous magnesium sulfate to remove moisture, filtered, and concentrated under reduced pressure. The residue obtained in this way was separated and purified by flash column chromatography to obtain 40.1 g of intermediate product C-1-4. |
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