Purification method of 2-methyl-4-isothiazolin-3-ketone
A technology of isothiazoline and purification method, which is applied in organic chemistry and other fields, and can solve problems such as low purity
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Example Embodiment
[0023] Example 1 of the purification method of 2-methyl-4-isothiazolin-3-one
[0024] The purification method of 2-methyl-4-isothiazolin-3-one in this embodiment includes the following steps:
[0025] (1) Mix 25g of 2-methyl-4-isothiazolin-3-one reagent (purity of 95%, purchased from Aladdin) with 10 mL of acetone (chromatographic purity of 99.8%, purchased from Merck), and heat up At 40°C, stir until completely dissolved, keep for 10 minutes, and filter to obtain a mixed solution.
[0026] (2) Place the mixed solution in a 25°C environment to cool naturally for 3 hours, then place it in a 4°C environment to cool for 5 hours, and then perform suction filtration to obtain crystals.
[0027] (3) Wash the crystals 3 times with petroleum ether.
[0028] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is nitrogen.
[0029] (4) Vacuum freeze-dry the washed crystals at -80℃ and vacuum degree <0.12Mbar, the drying time is 2 days, and finally 19.8g...
Example Embodiment
[0030] Example 2 of the purification method of 2-methyl-4-isothiazolin-3-one
[0031] The purification method of 2-methyl-4-isothiazolin-3-one in this embodiment includes the following steps:
[0032] (1) Mix 25g of 2-methyl-4-isothiazolin-3-one reagent (95% purity, Bailingwei Technology) with 25mL ethyl acetate (chromatographic purity 99.9%, purchased from Merck), and heat up To 50°C, stir until completely dissolved, keep for 20 minutes, and filter to obtain a mixed solution.
[0033] (2) Place the mixed solution in an environment of 20°C for natural cooling for 3 hours, then place it in an environment of 8°C for 5 hours and then perform suction filtration to obtain crystals.
[0034] (3) Wash the crystals 3 times with petroleum ether.
[0035] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is argon.
[0036] (4) Vacuum freeze-dry the washed crystals at a temperature of -40℃ and a degree of vacuum <0.12Mbar, the drying time is 4 days, an...
Example Embodiment
[0037] Example 3 of the purification method of 2-methyl-4-isothiazolin-3-one
[0038] The purification method of 2-methyl-4-isothiazolin-3-one in this embodiment includes the following steps:
[0039] (1) Mix 25g of 2-methyl-4-isothiazolin-3-one reagent (95% purity, Bailingwei Technology) with 25mL ethyl acetate (chromatographic purity 99.9%, purchased from Merck), and heat up To 45°C, stir until completely dissolved, keep for 15 minutes, and filter to obtain a mixed solution.
[0040] (2) Place the mixed solution in a 23°C environment to cool naturally for 3 hours, then place it in a 0°C environment to cool for 5 hours, and then perform suction filtration to obtain crystals.
[0041] (3) Wash the crystals 3 times with petroleum ether.
[0042] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is nitrogen.
[0043] (4) Vacuum freeze-dry the washed crystals at -80℃ and vacuum degree <0.12Mbar, the drying time is 4 days, and finally 21.2g of w...
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