A kind of synthetic method of 9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide
A synthesis method, phosphaphenanthrene technology, applied in the field of synthesis of 9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide, can solve OPP oxidation and volatilization, long reaction time, It is difficult to increase the reaction temperature to achieve the effects of short reaction cycle, avoiding oxidation and volatilization, and high yield
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Embodiment 1
[0026] Synthesis of tri-o-phenylphenyl phosphite:
[0027] At 90°C, 4.4 mL of PCl 3 Slowly drop it into 30.0 g of OPP, and then raise the temperature to 95°C to react for 2.5 hours. Excess OPP was distilled off under reduced pressure to obtain 26.4 g of tri-o-phenylphenyl phosphite.
[0028] Synthesis of CDOP:
[0029] 0.2g ZnCl 2 Add the obtained tri-o-phenylphenyl phosphite and raise the temperature to 180°C, slowly add 10.6mL of PCl dropwise within 2 hours 3 . After dripping, react for 3 hours, excess PCl 3 Removal under reduced pressure yielded 34.1 g of a yellow viscous CDOP melt.
[0030] Synthesis of HPPA:
[0031] The CDOP melt was cooled to 80°C, slowly added dropwise into 200mL 10% sodium hydroxide solution, and ice cubes were added to keep the temperature not exceeding 40°C. Add active carbon after dripping, and filter after stirring for 3 hours. The filtrate was neutralized to pH=4 with 50 mL of 37% concentrated hydrochloric acid, a large amount of white s...
Embodiment 2
[0035] Synthesis of tri-o-phenylphenyl phosphite:
[0036] At 95°C, 4.4 mL of PCl 3 Slowly drop it into 42.5g of OPP, and then raise the temperature to 100°C to react for 1.5 hours. Excess OPP was distilled off under reduced pressure to obtain 26.7 g of tri-o-phenylphenyl phosphite.
[0037] Synthesis of CDOP:
[0038] 0.2g ZnCl 2 Add the obtained tri-o-phenylphenyl phosphite and raise the temperature to 180°C, slowly add 10.6mL of PCl dropwise within 3 hours 3 . After dripping, react for 3 hours, excess PCl 3 Removal under reduced pressure yielded 34.5 g of a yellow viscous CDOP melt.
[0039] Synthesis of HPPA:
[0040] The CDOP melt was cooled to 80°C, slowly added dropwise into 200mL 10% sodium hydroxide solution, and ice cubes were added to keep the temperature not exceeding 40°C. Add active carbon after dripping, and filter after stirring for 3 hours. The filtrate was neutralized to pH=4 with 50 mL of 37% concentrated hydrochloric acid, a large amount of white s...
Embodiment 3
[0044] Synthesis of tri-o-phenylphenyl phosphite:
[0045] At 90°C, 4.4 mL of PCl 3 Slowly drop it into 25.5g of OPP, and then raise the temperature to 105°C to react for 2 hours. Excess OPP was distilled off under reduced pressure to obtain 26.1 g of tri-o-phenylphenyl phosphite.
[0046] Synthesis of CDOP:
[0047] 0.2g ZnCl 2 Add the obtained tri-o-phenylphenyl phosphite and raise the temperature to 160°C, slowly add 8.8 mL of PCl dropwise within 2 hours 3 . After dripping, react for 4 hours, excess PCl 3 Removal under reduced pressure yielded 33.1 g of a yellow viscous CDOP melt.
[0048] Synthesis of HPPA:
[0049] The CDOP melt was cooled to 80°C, slowly added dropwise into 200mL 10% sodium hydroxide solution, and ice cubes were added to keep the temperature not exceeding 40°C. Add active carbon after dripping, and filter after stirring for 3 hours. The filtrate was neutralized to pH=4 with 50 mL of 37% concentrated hydrochloric acid, a large amount of white sol...
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