In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Diphenyl oxide, other downstream synthetic routes, hurry up and to see.
Reference of 101-84-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 101-84-8, name is Diphenyl oxide belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
EXAMPLE 6; Preparation of Partially brominated DPO[0056] To the 500 mL flask (equipped as described in Example 4) containing 47.3 g of DPO was added over about 10 minutes, 28.0 g of bromine with stirring and cooling at room temperature. Catalyzed Bromination [0057] In a 1 -liter jacketed flask equipped with mechanical stirrer, Friedrich condenser(water cooled at about 250C), and with a 1/32-inch diptube but without a fractionation column were placed 3.8 g of AlCl3 and 885 g of bromine. After a feed time of about 7.25 hours, all of the partially brominated DPO had been fed from the flask. The reaction temperature was maintained at 56.30C to 57.20C throughout the addition. The reaction mixture was refluxed for 4 minutes as the temperature rose to 58.40C, then 450 mL of water was added and the reactor was set for distillation. The product was distilled to 1700F (about 770C) and 312 g of bromine was collected. The water layer was decanted from the reactor, 400 mL of water was added, stirred, and discarded. Then 400 mL of water and 10 g of NaOH were added, the mixture was stirred well and product was collected and water washed on a filter. GC analysis showed the product was composed of 99.71% of decabromodiphenyl oxide, and 0.034 and0.259% of the first and second nonabromodiphenyl oxide isomers, respectively. The product was placed in a 1250C oven and after drying overnight weighed 252.0 g. EXAMPLE 7Preparation of Partially brominated DPO [0058] To the 500 mL flask (equipped as described in Example 4) containing 49.1 g of DPO was added over aboutlO minutes, 29.7 g of bromine. This was purged with nitrogen to remove HBr. Catalyzed Bromination[0059] In a 1 -liter jacketed flask equipped as in Example 6 (no fractionation column) were placed 3.8 g of AlCl3 and 884 g of bromine. The mixture was heated to 59C and a feed of the partially brominated DPO formed above was initiated. The feed through the 1/32-inch diptube was set at a rate of about 0.21 mL per minute. All the partially brominated DPO was added over 3 hours and 23 minutes, The reaction mixture had been maintained at a temperature of 56.10C to 57.10C throughout the addition time reflux was continued for about 10 more minutes as the temperature rose to 59.60C. Then 450 mL of water was added to the reaction mixture and the reactor was set for distillation. The mixture was distilled to 770C and 294.5 g of bromine was collected. The mixture was worked up as in Example 6. GC analysis of the product showed 99.59% of decabromodiphenyl oxide and 0.11% and 0.296% of first and second nonabromodiphenyl oxide peaks, respectively. Present in the product were a few “lumps”. One was removed and a GC showed it contained 99.61% of decabromodiphenyl oxide and 0.100 and 0.291% of the first and second nonabromodiphenyl oxide isomers, respectively. The product was oven dried. EXAMPLE 8Preparation of Partially brominated DPO [0060] To the 500 mL flask (equipped as in Example 4) containing 49.00 g of DPO was added 31.4 g of bromine over about 10 minutes. Then the mixture was purged with nitrogen. Catalyzed Bromination[0061] In a 1 -liter jacketed flask, equipped as in Example 6, were placed 3.82 g OfAlCl3 and 988 g of bromine The mixture was heated to 56.O0C and addition of the partially brominated DPO begun at a feed rate of about 0.18 mL per minute. This feed was maintained for a period of about 4 hours with the temperature fluctuating between 53.O0C and 54.O0C. The mixture was allowed to reflux for about another 7 minutes with the temperature reaching about 600C. Then, 450 mL of water was added to the reaction mixture and the reaction vessel was set for distilling bromine. The distillation was conducted to 770C whereby an amount of 400.2 g of bromine was recovered. Product was isolated as in Example 5 and oven dried. GC analysis showed 0.093% and 0.471% of the first and second nonabromodiphenyl oxide peaks, respectively, and 99.436% of decabromodiphenyl oxide. After drying over the weekend the product weighed 260.1 g.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Diphenyl oxide, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27776; (2008); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem