4-CHLORO-3-NITROBENZENEBORONIC ACID, PINACOL ESTER 98 synthesis
- Product Name:4-CHLORO-3-NITROBENZENEBORONIC ACID, PINACOL ESTER 98
- CAS Number:913836-26-7
- Molecular formula:C12H15BClNO4
- Molecular Weight:283.52
16588-24-2
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$6.00/1g
73183-34-3
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$6.00/5g
913836-26-7
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$79.00/1g
Yield:913836-26-7 92%
Reaction Conditions:
with (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride;potassium acetate in 1,4-dioxane at 110; for 3 h;Inert atmosphere;Temperature;
Steps:
1.1 step 1:
To a three-necked flask was added 5-bromo-2-chloronitrobenzene (11.8 g, 50.0 mmol). Bispinacolato borate (12.7 g, 50.0 mmol), potassium acetate (9.8 g, 100.0 mmol),1,4-dioxane (, 120 mL) and[1,1'-Bis(diphenylphosphino)ferrocene]dichloropalladium (1.8 g, 2.5 mmol).The reaction solution was heated under reflux with nitrogen gas at 110° C. for 3 hours.Cool to room temperature and remove the solvent by distillation under reduced pressure.The residue was dissolved in ethyl acetate (200 mL).Filter to remove solid impurities,The filtrate was washed with water (60 mL) saturated brine (60 mL), dried over sodium sulfate and filtered.The filtrate was spin-dried, and the crude product was purified by silica gel column chromatography (petroleum ether:ethyl acetate volume ratio = 10:1).A yellow solid was obtained, Compound 1 (13.0 g, 45.9 mmol, 92%).
References:
CN107383076,2017,A Location in patent:Paragraph 0005; 0008-0010
635-22-3
149 suppliers
$17.67/1gm:
73183-34-3
589 suppliers
$6.00/5g
913836-26-7
56 suppliers
$79.00/1g