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CAS No. : | 36692-49-6 | MDL No. : | MFCD00017098 |
Formula : | C8H10N2O2 | Boiling Point : | - |
Linear Structure Formula : | (CH3OCO)C6H3(NH2)2 | InChI Key : | IOPLHGOSNCJOOO-UHFFFAOYSA-N |
M.W : | 166.18 | Pubchem ID : | 135524 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P301+P312-P302+P352-P304+P340-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
68% | With potassium carbonate;copper; In chlorobenzene; for 20h;Heating / reflux; | A mixture of <strong>[181765-85-5]methyl 4-chloro-2-iodobenzoate</strong> (0.593g, 2 mmol), methyl 3,4- diaminobenzoate (0.332g, 2 mmol), copper (0.126g, 2 MMOL), and K2CO3 (0.276g, 2 mmol) in chlorobenzene (40 mL) was heated to reflux for 20 hours, cooled to room temperature, diluted with ethyl acetate, and filtered through diatomaceous earth (ELITE). The solution was washed with water and brine, dried (MGS04), filtered, and concentrated under vacuum. The residue was purified by flash column chromatography on silica gel with 7: 3 hexanes/ethyl acetate to provide 0.453g (68 %) of the desired product. MS (DCI) m/e 334 (M+H) +, 352 (M+NH4) + ; 1H NMR (300 MHz, DMSO-D6) # 8.99 (s, 1H), 7.89 (d, J = 8.5 Hz, 1 H), 7.47 (d, J = 1.0 Hz, 1H), 7.21 (m, 2H), 6.80 (dd, J = 8.5, 2.0 Hz, 1H), 6.65 (d, J = 2.1 Hz, 1H), 5.30 (s, 2H), 3.86 (s, 3H), 3.82 (s, 3H). |
With copper; potassium carbonate; In chlorobenzene; for 18h;Reflux; | Example 39Amethyl 2-(2-amino-4-(methoxycarbonyl)phenylamino)-4-chlorobenzoate To a solution of methyl-3,4-diaminobenzoate (2.8 g, 16.86 mmol, Alfa Aesar Chemical Company) in chlorobenzene (125 ml) was added Example 3A (5.0 g, 16.86 2345 mmol), K2CO3 (2.5 g, 17.71 mmol), and Cu (1.1 g, 16.86 mmol). The resulting mixture was heated at reflux over 18 hours. While hot, the mixture was filtered through a thin layer of diatomaceous earth and the cake washed with dichloromethane. The filtrate was concentrated and the crude product purified by flash chromatography on silica gel, eluting with a 10% - 100% CH2CI2 / hexanes gradient to yield the title compound. MS 2350 ESI(+) /M/Z 334.9 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With camphor-10-sulfonic acid; In ethanol; water; at 20℃; for 3h;Heating / reflux; | 2d 2-tert-butoxycarbonylamino-1H-benzimidazole-5-carboxylic acid Methyl 3,4-diaminobenzoate (7.0 g, 1 equivalent), <strong>[107819-90-9]1,3-bis(tert-butoxycarbonyl)-2-methyl-2-thiopseudourea</strong> (19.6 g, 1.6 equivalents) and camphorsulfonic acid (200 mg, cat.) are heated at reflux in ethanol (200 ml) for 3 h. The mixture is allowed to cool to r.t., then the solid is filtered, washed with ethanol, and dried to afford the intermediate methyl ester (8.2 g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With copper; potassium carbonate; In chlorobenzene; at 135℃; | Example 3Bmethyl 2-(2-amino-5-(methoxycarbonyl)phenylamino)-4-chlorobenzoate Example 3 A (3.0 g, 10.12 mmol), methyl-3,4-diaminobenzoate (3.39 g, 10.12 mmol), 2C03 (1.47 g, 10.63 mmol), Cu (0.648 g, 10.12 mmol) and chlorobenzene ( 100 1 735 ml) were mixed. The reaction mixture was heated to reflux ( 135C) overnight then filtered hot through a thin layer of diatomaceous earth. The flask was rinsed and the cake was washed with CH2CI2 (100 ml). The filtrate was washed with water, dried (Na^SC^), filtered and concentrated. The crude product was purified by column chromatography with an Analogix SF-150 g Si column using 90: 10 CH2CI2: hexanes (25 minutes) then 1740 100% CH2CI2 to yield the title compound. MS ESI(+) m/z 334.9 [M+H]+ |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.7% | In N,N-dimethyl-formamide; at 90.0℃; for 8.0h; | Take a 100ml single-mouth bottle,Add 3,4-diaminobenzoic acid methyl ester (2) 3.32 g (0.02 mol),And added 30 ml of N,N-dimethylformamide, and dissolved by stirring.Then, [1,4]dioxane-2,3-diol (a) 3.6 g (0.03 mol) was added.Stir at 90 C for 8 hours.Then extracted, washed,Drying to give methyl quinoxaline-6-carboxylate (3)3.64 g, yield 96.7%. |
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