4,4'-Dibromo-2,2'-diiodobiphenyl

A 17percent (w/w) HCl aqueous solution (85mL) at 0°C was added to the compound containing (Β-3) (8 ·5g, 25mmol) of Round-bottomed flask, and to this was added NaNO2 (NaNO2 solution [NaNO24.3g (62mmol) + water (15mL)] was added . The mixture was stirred for 30 minutes, and this was added an aqueous solution of KI [KI 41.5g (250_mmol) + water (15mL) ]. the mixture was stirred at room temperature for 1 hour, at 60 ° C and stirred for 3 hours. K0H with a saturated solution and extracted with ethyl acetate and washed with saturated Na2SO3 (V Dr Di, the residue was purified by column chromatography to give compound B-4 (4g, 29percent).At a temperature of about 0° C., 85 mL of a 17percent (w/w) HCl aqueous solution and a NaNOTo a round bottom flask containing 8.5 g (25 mmol) of the compound B-3 at 0 °C was added 85 mL of 17percent (w/w) aqueous HCl solution and an aqueous solution of NaNO2 [4.3 g (62 mmol) of NaNO2 + 15 mL of water] was added. Stirred for 30 minutes and KI aqueous solution [KI 41.5 g (250 mmol) + water 15 mL] was added. Stirred at room temperature for 1 hour and stirred at 60 °C for 3 hours. The reaction mixture was neutralized with saturated KOH solvent, extracted with ethyl acetate, washed with saturated Na2SO3 and then purified by silica column to obtain 4 g (29percent) of compound B-4.Step ^ - Preparation of Compound Int-43bTo a stirred suspension of 2, 2'-diamino-4, 4'-dibromobiphenyl Int-43a (11.2 g, 33 mmol) (prepared from J. Am. Chem. Soc. 2005, 127, 7662) in cone. HC1 (50 mL)/water (50 mL) at 0 °C was added a 50percent soln of NaN0(3) The compound 3 (7.16 g, 20 mmol) and p-toluenesulfonic acid (17.18 g, 90.4 mmol) were dissolved in 200 mL of acetonitrile, stirred at 0 ° C for half an hour, and sodium nitrite (4.14, 1) and potassium iodide (12.45 g, 75 mmol) were dissolved in 40 mL of water and added dropwise to the reaction flask with a constant pressure dropping funnel, which was then allowed to warm to room temperature and allowed to react overnight. After completion of the reaction, the saturated sodium thiosulfate solution was added to the reaction solution and the resulting iodine was extracted and extracted with methylene chloride. The organic phase was collected and dried over anhydrous sodium sulfate. The product was purified by silica gel chromatography using petroleum ether as eluent The residue was purified by column chromatography and dried in vacuo to give a white solid 4 in a yield of 25percent

Molecular Weight:563.79
XLogP3:6.2
Rotatable Bond Count:1
Exact Mass:563.69052
Monoisotopic Mass:561.69257
Heavy Atom Count:16
Complexity:213
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes