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CAS No. : | 201227-39-6 | MDL No. : | MFCD07371567 |
Formula : | C8H4BrN3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | QIULWQLXNFSZJG-UHFFFAOYSA-N |
M.W : | 222.04 | Pubchem ID : | 24728911 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
60% | To a cooled solution of (2-amino-5-bromophenyl)acetonitrile (11 g, 52 mmol) in concentrated hydrochloric acid (110 mL) at -50 C., a solution of sodium nitrite (3.9 g, 57 mmol) in water (20 mL) was added slowly. After the addition, the mixture was stirred at -50 C. for 2 h. The mixture was neutralized with 33% ammonium hydroxide at 0 C. and extracted with ethyl acetate (3*100 mL). The combined organic layers were washed with saturated sodium chloride (100 mL), dried over anhydrous sodium sulfate and concentrated. The obtained crude product was purified by column chromatography (100-200 mesh silica gel) using 10% ethyl acetate in petroleum ether as eluent to afford 5-bromo-3-cyanoindazole (7 g, 60%) as a solid. 1HNMR (CDCl3) δ ppm 10.7 (br, 1H), 8.1 (s, 1H), 7.64 (d, 1H), 7.5 (d, 1H). | |
60% | With hydrogenchloride; sodium nitrite; In water; at -50℃; for 2h; | To a cooled solution of (2-amino-5-bromophenyl)acetonitrile (11 g, 52 mmol) in concentrated hydrochloric acid (110 mL) at -50 C, a solution of sodium nitrite (3.9 g, 57 mmol) in water (20 mL) was added slowly. After the addition, the mixture was stirred at-50 C for 2h. The mixture was neutralized with 33% ammonium hydroxide at 0 C and extracted with ethyl acetate (3x100 mL). The combined organic layers were washed with saturated sodium chloride (100 mL), dried over anhydrous sodium sulfate and concentrated. The obtained crude product was purified by column chromatography (100-200 mesh silica gel) using 10% ethyl acetate in petroleum ether as eluent to afford 5-bromo-3-cyanoindazole (7 g, 60%) as a solid. 1HNMR (CDCIs) ppm 10.7 (br, 1 H), 8.1 (s, 1 H), 7.64 (d, 1 H), 7.5 (d, 1 H). |
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