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CAS No. : | 583-75-5 | MDL No. : | MFCD00007825 |
Formula : | C7H8BrN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | PCHYYOCUCGCSBU-UHFFFAOYSA-N |
M.W : | 186.05 | Pubchem ID : | 11423 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
With 2 wt% Pd/C; hydrogen; at 120℃; under 7500.75 Torr; | Examples 27 to 34 investigated the effect of carbon-supported large-particle palladium catalysts on the synthesis of halogenated aromatic amines by solvent-free hydrogenation of different halogenated aromatic nitro compounds. In a 500 ml reactor, 200 g of different halogenated aromatic nitro compounds were added, 2 g of a 2 wt% palladium catalyst containing a large particle size in Example 5, shutting down the reactor; first with nitrogen replacement reactor inside the air three times, and then replaced with hydrogen three times, And then heated to 120 C, and the hydrogen pressure rose to 1MPa, open stirring to 1000r/min; to maintain the reaction temperature and pressure until the end of the reaction; cooling cooling, remove the reactor liquid, filter separation The catalyst was used and the water in the filtrate was separated by phase separation to give the desired product Halogenated aromatic amine. The reaction product was analyzed by gas chromatography. The results are shown in Table 4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | With dihydrogen peroxide; trifluoroacetic anhydride; In dichloromethane; at 0℃; for 1.58333h;Heating / reflux; | Example 37; 2-methoxy-N-(2-methyl-4-(1-(2-(methylamino)ethyl)piperidin-4-yl)phenyl)benzamide (199); Step 1 4-bromo-2-methyl-1 -nitrobenzene (193); [0383] To a mixture of H2O2 (3 95 ml, 64 5 mmol) in DCM (32 0 ml) cooled at O 0C was added TFAA (10 93 ml, 77 mmol) and the mixture was stirred for 5 minutes at that temperature then the ice bath was removed and a reflux condenser was installed and a solution of 4-bromo-2-methylaniline (3 g, 16 12 mmol) in DCM (6 4 ml) was added drop-wise over approx 30 minutes The reaction was heated at reflux for an additional hour then it it was cooled, washed with 30 mL of water then 30 mL of sat NaHCO3 and the organic layer was dried over MgSO4 and concentrated under vacuum The crude material was purified by flash to afford 193 (2 57 g, 1 1 9 mmol, 74%) 1H NMR (CDCI3) delta (ppm) 7 88 (d, J = 8 6 Hz, 1 H),7 53 (d, J = 2 2 Hz, 1 H), 7 49 (dd, J = 8 6, 2 2 Hz, 1 H), 2 60 (s, 3H) |
With sulfuric acid; dihydrogen peroxide; In hexane; water; acetic acid; | Step A: Preparation of 5-bromo-2-nitrotoluene A solution of 4-bromotoluidine (27.9 g, 150 mmoles) in glacial acetic acid (600 ml) is stirred while 30% hydrogen peroxide (180 ml) and concentrated sulfuric acid (12 ml) are added. The mixture is heated in an oil bath at 100. When the pot temperature reaches 65 the mixture darkens and there is a mild exotherm. The bath is removed and the temperature rises to 105. When the reaction subsides, the bath is replaced and reflux is maintained for two hours. The mixture is cooled and poured onto ice (1500 g). The product crystallizes slowly with scratching. Another liter of cold water is added and the product is filtered and washed. The damp solid is dissolved in hexane, filtered, dried and evaporated to a residue which crystallizes to give 14.3 g of 5-bromo-2-nitrotoluene, containing minor contaminants by tlc [silica gel-dichloromethane/hexane (3:7)] which were removed by column chromatography using the same solvent system. Final weight; 12.8 g. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: Catalytic reaction was carried out in a 50 mL two necked round bottom flask, which charged with 0.05 g of catalyst, substrate (2 mmol) in acetic acid (5 mL) and KBr (2.2 mmol). 30% H2O2 (2.2 mmol) was then added drop wise to the reaction mixture. The content in the flask was stirred continuously at room temperature. After specified time of the reaction, the catalyst was filtered and the solid was washed with ether. The combined filtrates were washed with saturated sodium bicarbonate solution and then shaken with ether in a separating funnel. The organic extract was dried over anhydrous sodium sulfate. The products were analysed by Varian 3400 gas chromatograph equipped with a 30 m CP-SIL8CB capillary column and a Flame Ionization Detector. Identity of the products was also confirmed by using an Agilent GC-MS. |
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