Method for preparing 1,1-cyclopropanedimethyl cyclicsulfite
A technology of methanol cyclic sulfite and body cyclic sulfite, applied in the field of preparation 1, can solve the problems of high cost, cumbersome processing, many reaction steps, etc., and achieves low cost, high reaction yield, and is beneficial to industrial production. Effect
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Embodiment 1
[0042] A method for preparing 1,1-cyclopropane dimethanol cyclosulfite, the specific steps are:
[0043] Step 1, synthetic intermediate cyclic sulfite, its general reaction chemical formula is as follows:
[0044]
[0045] Specifically: after mixing dibromoneopentyl glycol (200 g, 0.76 mol) with 350 ml of toluene, heat to 40° C.;
[0046] Thionyl chloride (100 g, 0.84 moles) was added dropwise, and the temperature of the solution rose to above 45° C. due to the mild exothermic reaction. At this time, the reaction temperature was maintained at 45° C. to 55 °C, drop the thionyl chloride in about 1 hour; during the reaction, use lye to absorb the hydrogen chloride (HCl) gas generated after the solid gradually dissolves;
[0047] Then the reaction mixture was heated to 50°C for 2.5 hours;
[0048] After completion of the reaction, the toluene solution was evaporated to dryness under reduced pressure, and the obtained oily liquid solidified after cooling and standing; after th...
Embodiment 2
[0055] A method for preparing 1,1-cyclopropane dimethanol cyclosulfite, the specific steps are:
[0056] Step 1, synthetic intermediate cyclic sulfite, its general reaction chemical formula is as follows:
[0057]
[0058] Specifically: after mixing dibromoneopentyl glycol (200 g, 0.76 mol) with 350 ml of toluene, heat to 40° C.;
[0059] Thionyl chloride (100 grams, 0.84 moles) was added dropwise, and the temperature of the solution rose to above 45°C due to the mild exothermic reaction. °C, drop the thionyl chloride in about 1 hour; during the reaction, use lye to absorb the hydrogen chloride (HCl) gas generated after the solid gradually dissolves;
[0060] Then the reaction mixture was heated to 50°C for 2.5 hours;
[0061] After the reaction was completed, the toluene solution was evaporated to dryness under reduced pressure, and the obtained oily liquid solidified after cooling and standing; after the obtained solid was pulverized, washed with water (1 liter × 3), fi...
Embodiment 3
[0068] A method for preparing 1,1-cyclopropane dimethanol cyclosulfite, the specific steps are:
[0069] Step 1, synthetic intermediate cyclic sulfite, its general reaction chemical formula is as follows:
[0070]
[0071] Specifically: after mixing dibromoneopentyl glycol (200 g, 0.76 mol) with 350 ml of toluene, heat to 40° C.;
[0072] Thionyl chloride (100 grams, 0.84 moles) was added dropwise, and the temperature of the solution rose to above 45°C due to the mild exothermic reaction. °C, drop the thionyl chloride in about 1 hour; during the reaction, use lye to absorb the hydrogen chloride (HCl) gas generated after the solid gradually dissolves;
[0073] Then the reaction mixture was heated to 50°C for 2.5 hours;
[0074] After the reaction was completed, the toluene solution was evaporated to dryness under reduced pressure, and the obtained oily liquid solidified after cooling and standing; after the obtained solid was pulverized, washed with water (1 liter × 3), fi...
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