Synthesis method of 1, 4-dioxane-2, 5-diol
A dioxane and synthesis method technology, applied in the direction of organic chemistry, etc., can solve problems such as complex operation procedures, expensive raw materials, difficult post-processing, etc., and achieve simple operation steps and post-processing, improved yield, and low price Effect
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Embodiment 1
[0033] Add 500g of chloroacetaldehyde with a mass fraction of 10% in the three-necked flask, then add 66g of solid sodium bisulfite, start stirring, heat up to dissolve, control the reaction temperature to 40°C, keep the reaction for 4 hours, and cool down after the reaction is completed , drop hydrochloric acid to adjust its pH value to 2, precipitate chloroacetaldehyde ω-sulfonic acid solid, cool down to about 10°C, and centrifugally filter to obtain chloroacetaldehyde ω-sulfonic acid wet product 145g (about 44g in water).
[0034] Then add 145g of chloroacetaldehyde omega-sulfonic acid wet product into another three-necked flask, add 23g of water, add 297g of sodium hydroxide with a mass fraction of 30%, heat up to 90°C for 3 hours, and then heat to reflux for 5 hours After the end of the reaction was detected by TLC, the distillation device was changed. When the material became thick, 100g of toluene was added for azeotropic dehydration. After the water was completely remov...
Embodiment 2
[0036] Add 125g of chloroacetaldehyde with a mass fraction of 40% in the three-necked flask, then add 66g of solid sodium bisulfite, start stirring, heat up to dissolve, control the reaction temperature to 42°C, keep the reaction for 5 hours, and cool down after the reaction is completed , hydrochloric acid was added dropwise to adjust its pH value to 3, and the chloroacetaldehyde ω-sulfonic acid solid was precipitated, cooled to about 5°C, and centrifugally filtered to obtain 133 g of chloroacetaldehyde ω-sulfonic acid wet product (about 32 g in water).
[0037] Then 133g of chloroacetaldehyde omega-sulfonic acid wet product was added in another three-necked flask, 23g of water was added, 297g of sodium hydroxide with a mass fraction of 30% was added, the temperature was raised to 80°C for 4 hours, and then heated to reflux for 6 hours. After the end of the reaction was detected by TLC, the distillation device was changed. When the material became thick, 100g of toluene was ad...
Embodiment 3
[0039] Add 250g of chloroacetaldehyde with a mass fraction of 20% in the three-necked flask, then add 66g of solid sodium bisulfite, start stirring, heat up to dissolve, control the reaction temperature to 42°C, keep the reaction for 5 hours, and cool down after the reaction is completed , drop hydrochloric acid to adjust its pH value to 3, precipitate chloroacetaldehyde ω-sulfonic acid solid, cool to about 5°C, and centrifugally filter to obtain chloroacetaldehyde ω-sulfonic acid wet product 139g (about 38g in water).
[0040] Then 139g of chloroacetaldehyde omega-sulfonic acid wet product was added in another three-necked flask, 23g of water was added, 297g of sodium hydroxide with a mass fraction of 30% was added, the temperature was raised to 80°C for 4 hours, and then heated to reflux for 6 hours. After the end of the reaction was detected by TLC, the distillation device was changed. When the material became thick, 100g of toluene was added for azeotropic dehydration. Afte...
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