Method for synthesizing 9, 10-dihydro-9-oxygen-10-phosphaphenanthrene-10-oxide
A synthesis method, the technology of phosphaphenanthrene, which is applied in the field of synthesis of 9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide, can solve the problem of difficulty in increasing the reaction temperature, OPP oxidation and volatilization, Avoiding oxidation and volatilization, short reaction cycle 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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