Related Products of 117635-21-9,Some common heterocyclic compound, 117635-21-9, name is 1,4-Dibromo-2,5-dihexylbenzene, molecular formula is C18H28Br2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In the dry box the mixture of boronic acid 5, (3.69g, 15.58mmol), 1 ,4- dibromo-2,5-dihexylbenzene (3.15g, 7.8mmol), Aliquat 336 (0.8g),Pd(PPh3) (0.858g, 0.742mmol) in degassed toluene (50ml_) was prepared. Outside dry box, the degassed Na2CO3 (3.93g, 37.1 1 mmol in 50 ml_ of water) solution was added to the former mixture under nitrogen, and then the resultant mixture was stirred at 90C for 18hrs. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over anhydrous MgSO4. Filtration, concentration of the filtrate, and then the silica columnchromatography (10-50% DCM in hexane) provided the desired product (3.7g, 80% yield) as a solid. This diboc-protected material wasdeprotected by the overnight reaction at room temperature with TFA solution (2ml_ of TFA in 50ml_ of DCM). The reaction mixture was concentrated under reduced pressure followed by the neutralization with saturated NaHCO3. Ethyl acetate extraction, drying over anhydrous MgSO4, concentration of the organic layer under reduced pressure, then silica column chromatography (10-50% ethyl acetate in hexane) provided the desired diamine material, 6, (1 .89g, 75% yield) as a viscous liquid.
The synthetic route of 117635-21-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; PARK, Kyung-Ho; RADU, Nora, Sabina; JOHANSSON, Gary, A.; FENNIMORE, Adam; DELANEY, William, J.; LECLOUX, Daniel, David; WO2011/159872; (2011); A1;,
Bromide – Wikipedia,
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