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CAS No. : | 625446-22-2 | MDL No. : | MFCD03411551 |
Formula : | C8H6BrFO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ASKFCSCYGAFWAB-UHFFFAOYSA-N |
M.W : | 217.04 | Pubchem ID : | 21938581 |
Synonyms : |
|
Chemical Name : | 1-(4-Bromo-2-fluorophenyl)ethanone |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H319 | 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 |
---|---|---|
72% | With hydrazine hydrate; In ethylene glycol; at 165℃; for 12h; | Intermediate 95 6-bromo-3-methyl-1H-indazole To a solution of intermediate 94 (3.7 g, 17.04 mmoles) in 1,2-ethanediol (25 ml), hydrazine hydrate (1.65 ml, 34.09 mmoles) was added at room temperature and heated to 165 C. After 12 h, the reaction mixture cooled to room temperature, quenched with water and solid precipitated was filtered and dried under vacuum to afford the title compound as colourless solid (2.5 g, 72% yield). 1H-NMR (delta ppm, DMSO-d6, 400 MHz): delta 12.74 (s, 1H), 7.67 (d, J=5.8 Hz, 1H), 7.65 (s, 1H), 7.19 (dd, J=8.6, 1.4 Hz, 1H), 2.46 (s, 3H). |
With hydrazine hydrate; In ethylene glycol; at 20 - 200℃; for 1.5h;Microwave irradiation; | Part C: Compound 721 (1.1 g, 5.04 mmol) was dissolved in ethylene glycol (10 ml_) and hydrazine monohydrate (277 mg, 5.5 mmol) and stirred at room temperature for 30 minutes followed by 1 hour at 200 0C in a microwave. The reaction was quenched with brine and extracted with methylene chloride. The organic layer was dried over sodium sulfate and concentrated to provide compound 722 (1.0 g). 1H NMR (400 MHz, CDCI3): delta 7.65 (m, 1 H), 7.58 (m, 1H), 7.3 (m, 1 H), 2.6 (S, 3H). | |
With hydrazine hydrate; In ethanol; at 120℃; for 23h; | Intermediate 125; 6-Bromo-3-methyl-1 H-indazole; A suspension of 1-(4-bromo-2-fluorophenyl)ethanone (8.33 g, 38.4 mmol) in 15 mL of hydrazine monohydrate (309 mmol, 8 equiv) was heated to 120 0C under a reflux condenser for 23 hours. The resulting suspension (after cooling to room temperature) was filtered. The white solids were washed with water (2 X 15 mL), sucked under house vacuum at room temperature for 24 hours, and then dried under vacuum at room temperature over P2O5 for 24 hours to afford the title compound (7.59 g) as a yellow solid. LC-MS (ES) m/z = 211 , 213 [M+H]+. |
With hydrazine hydrate; In ethylene glycol; at 200℃; for 4.5h;Microwave irradiation; | [0001196] To a solution of l-(4-bromo-2-fluorophenyl)ethan-l-one (1.0 g, 3.89 mmol) in 1 ,2-ethanediol (12 mL) was added 80% of hydrazine monohydrate (0.6 mL, 7.78 mmol) at room temperature. The reaction mixture was stirred at 200 C in a microwave for 4.5 h, cooled down to room temperature, and quenched with water (50 mL). The solid precipitated was filtered, washed with water (20 mL), and dried under vacuo to afford Compound 334A. | |
With hydrazine hydrate; In ethanol; at 120℃; for 12h; | [000673j A stirred solution of compound 3 (1 eq) in hydrazine monohydrate (8 eq) was stirred at 120 C for 12 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was diluted with water, extracted with ethyl acetate (3 X 25 mL). The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The crude product was washed with diethyl ether to afford compound 4. LCMS (mlz): 213.00 (M+2). |
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