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Type | HazMat fee for 500 gram (Estimated) |
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Structure of 33720-71-7
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The BI-3802 was designed by Boehringer Ingelheim and could be obtained free of charge through the Boehringer Ingelheim open innovation portal opnMe.com, associated with its negative control.
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Batch number can be found on the product's label following the word 'Batch'.
Search for reports by entering the product batch number.
Batch number can be found on the product's label following the word 'Batch'.
Search for reports by entering the product batch number.
Batch number can be found on the product's label following the word 'Batch'.
Search for reports by entering the product batch number.
Batch number can be found on the product's label following the word 'Batch'.
Search for reports by entering the product batch number.
Batch number can be found on the product's label following the word 'Batch'.
CAS No. : | 33720-71-7 |
Formula : | C9H8N2O |
M.W : | 160.17 |
SMILES Code : | N#CC1=CC(C(C)=O)=CC=C1N |
MDL No. : | MFCD18379155 |
InChI Key : | SJXQSPLLUXAJQJ-UHFFFAOYSA-N |
Pubchem ID : | 10866627 |
GHS Pictogram: |
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Signal Word: | Danger |
Hazard Statements: | H301+H311+H331-H315-H319-H317 |
Precautionary Statements: | P501-P261-P272-P270-P271-P264-P280-P337+P313-P305+P351+P338-P361+P364-P333+P313-P301+P310+P330-P302+P352+P312-P304+P340+P311-P403+P233-P405 |
Class: | 6.1 |
UN#: | 3439 |
Packing Group: | Ⅲ |
* 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 |
---|---|---|
94.8% | With copper(ll) bromide; In tetrahydrofuran; for 4.0h;Heating / reflux; | c.. Preparation of 3-cyano-4-amino-alpha-bromo-acetophenone The mixture of 20.0g of 3-cyano-4-amino-acetophenone and 54.28g of copper bromide in 300ml of THF was refluxed for 4h, cooled, and filtered at room temperature.. The filtrate was distilled in vacuo to remove THF. The residue was washed with small amount of ethanol to give title product as yellow solid.. Yield 94.8%; melting point 160-161 C.(decomp.). |
80% | With copper(ll) bromide; In ethanol; chloroform; ethyl acetate; for 2.0h;Reflux; | Weigh 2.8 g (17.5 mmol) of <strong>[33720-71-7]4-amino-3-cyanoacetophenone</strong> in a 250 ml round bottom flask and add 60 ml of EA, 60 ml.CHCl3 and 20ml CH3CH2OH solvent at reflux temperatureStir and dissolve. Weigh 7.8 g (35 mmol) of copper bromide,After adding the reaction device, refluxing for 2 hours, the mixture was filtered while hot, and the filtrate was collected, washed three times with 20 ml of water each time, and the organic phase was collected.After drying over anhydrous sodium sulfate, the solvent was evaporated to dryness to give 4-amino-3-cyanobromoacetophenone 3.4 g (yield: 80%). |
With copper(ll) bromide; In ethyl acetate; for 4.0h;Reflux; | [0370] Step 2: <strong>[33720-71-7]5-acetyl-2-aminobenzonitrile</strong> (523 mg) and copper (II) bromide (1.00 g) were added to ethyl acetate (20 ml). After the mixture was refluxed for 2 hours, additional copper (II) bromide (500 mg) was added and further refluxed for 2 hours. The mixture was cooled to room temperature and filtered through a celite pad. The resulting filtrate was washed with a sodium hydrogen carbonate aqueous solution and a saturated sodium chloride solution, and dried over sodium sulfate. The solution was evaporated under reduced pressure, thereby obtaining crude 2-amino-5-(2-bromoacetyl)benzonitrile (360 mg). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56.9% | In DMF (N,N-dimethyl-formamide); for 6.0h;Heating / reflux; | b.. Preparation of 3-cyano-4-amino-acetophenone The 3-iodo-4-amino-acetophenone as prepared above was dissolved 95ml of DMF and 20.9g CuCN was added.. Stirred under reflux for 6h and cooled down to 100C. The reaction mixture was poured into 2L of water, and cooled.. The precipitate was filtered off, air dried and extracted with THF. Evaporated, washed with ethanol, filtered, and dried to give product as yellow crystal.. Yield 56.9%; melting point 150-152C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | After suction filtering and washing of the filter residue with water and drying this residue at 60 C., 21 g of beige 3-cyano-4-aminoacetophenone is obtained, corresponding to a yield of 87.5% of theory. Melting point: 161.5 C. If sodium hydroxide and methanol are used in the same molar ratios and under the same reaction conditions, 3-cyano-4-aminoacetophenone is obtained in a yield of 80% of theory. |
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