The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 101-84-8, name is Diphenyl oxide, A new synthetic method of this compound is introduced below., name: Diphenyl oxide
EXAMPLE 1; Catalyzed Bromination [0047] A reactor was configured from a 1 -liter Morton flask with a mechanical stirrer, thermometer, 60 mL addition funnel, and fractionation column (10″ x 1″ (ca. 25.4 cm x 2.54 cm) with 5 mm x 5 mm Raschig rings) topped by a O0C reflux condenser. The outlet of the condenser was connected to a H2O trap. A small N2 purge was added to the line from the condenser to the H2O trap. The reactor was charged with 3.5 g OfAlCl3 and 1577g of bromine (containing 11 ppm H2O). The addition funnel was charged with 47.04 g of diphenyl oxide.The reactor was heated to 550C and the diphenyl oxide was added drop-wise supersurface. The time for the initiation of the diphenyl oxide addition was noted. The reactor was heated by a mantle. Twenty-seven minutes into the diphenyl oxide feed, half of the diphenyl oxide had been added and the reaction mass temperature was 560C. One and a quarter hours after the diphenyl oxide feed was initiated, all of the diphenyl oxide had been added and the reaction mass temperature was 570C. The compressor on the refrigeration system was shut off to allow slow warm-up of the condenser. The reaction mass was refluxed through the fractionation column. At one hour and 18 minutes after feed initiation, the reaction mass temperature was 590C. Two hours and three minutes after diphenyl oxide feed initiation the condenser water was at 2O0C and the reaction temperature was at 610C. At two hours and seven minutes after feed initiation, the condenser water was at 3O0C. Thirty two minutes later the addition funnel was replaced with a N2 inlet. A slow N2 purge of the reactor was started. The reaction mass temperature was 610C. The N2 purge was at 100 mL/min into the vapor space of the reactor. Four hours and fifty minutes after the initiation of the diphenyl oxide feed, the reaction mass temperature was 610C and the condenser water was at 370C. At six hours and 15 minutes after the initiation of the diphenyl oxide feed the reaction mass was cooled to 550C, 350 mL deionized H2O was added, the fractionation column was removed, and the reactor was set for distillation. Br2 was distilled off. When most of the Br2 was gone 150 mL more deionized water was added. The remaining Br2 was distilled off to 1000C. The remaining mixture was cooled to 6O0C, and 30 mL of 25% NaOH was added to pH 13-14. The resultant mix was filtered and washed well with deionized water. A sample was subjected to GC analysis. The GC trace showed the product to contain 0.21% of the first nonabromodiphenyl oxide peak (deemed to be meta- and para-hydrogen isomers), 0.24% of the second nonabromodiphenyl oxide peak (deemed to be the ortho-hydrogen isomer) and 99.54% of decabromodiphenyl oxide. The sample was oven dried.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27776; (2008); A2;,
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