Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore
A technology of nitrophenoxy and nitrotrifluoromethylbenzene, which is applied in the field of hexafluoropropane preparation, can solve the problems of unfavorable environmental protection, increase of three wastes, increase of chemical unit operations, etc., and achieve convenient source of raw materials and variety of uses The effect of less and simplified process
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Embodiment 1
[0025] 33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 47.4 grams (0.21 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 27.6 grams (0.20 moles) of potassium carbonate, 410 milliliters of anhydrous N, N-dimethylformamide were put into the reaction kettle, stirred, heated to 110°C for 5 hours, continued to heat up to 140°C for 5 hours , filtered while it was hot, removed the filter residue, concentrated the mother liquor, recovered the solvent for recycling, cooled and stood still, and precipitated a milky white solid product, filtered, washed 2 to 3 times with pure water, and dried to obtain 69.9 grams of 2,2-bis[4 -(2-Trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product (theoretical yield is 71.4 g) with a purity of 99.5% and a melting point of 173.2°C-174.8 ℃ (WRR melting point apparatus, the initial setting temperature is 168 ℃, the heating rate is 1.0 ℃ / min), and its Fourier transform infrare...
Embodiment 2
[0028] 33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 56.4 grams (0.25 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 55.2 grams (0.40 moles) of potassium carbonate, 4490 milliliters of anhydrous N, N-dimethylacetamide were put into the reaction kettle, stirred, heated to 150° C. after reacting for 8 hours, filtered while hot, removed the filter residue, concentrated the mother liquor, The solvent was recovered for recycling, cooled and left to stand, and the milky white solid product was precipitated, filtered, washed 2 to 3 times with pure water, and dried to obtain 68.5 grams of 2,2-bis[4-(2-trifluoromethyl-4-nitrate phenyloxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product (theoretical yield: 71.4 g) with a purity of 99.0%.
[0029] According to the theoretical yield and the actual amount of 2,2-bis[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF), the calculated 2,2- The yield of bis[4-(2-...
Embodiment 3
[0031]33.6 grams (0.10 moles) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BHPFP), 45.1 grams (0.20 moles) of 2-chloro-5-nitrotrifluoromethylbenzene (CNB-TF) , 10.6 grams (0.10 moles) of sodium carbonate, and 600 milliliters of anhydrous N-methyl-2-pyrrolidone were put into the reaction kettle, stirred, heated to 130° C. for 5 hours, continued to heat up to 200° C. for 0.5 hours after the reaction, Filtrate while hot, remove the filter residue, concentrate the mother liquor, recover the solvent for recycling, cool and stand still, and precipitate a milky white solid product, filter, wash 2 to 3 times with pure water, and dry to obtain 65.7 grams of 2,2-bis[4-( 2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) milky white solid product with a purity of 99.2%.
[0032] Based on the amount of 2,2-bis[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl]hexafluoropropane (BNPFP-2TF) actually obtained and the theoretical yield (71.4 g), calculate The yield of 2,2-bis[4-...
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