Solid organic magnetic compound 3-chlorin bi-indene tetrone and synthetic method
A technology of chloroninhydrin and magnetic compounds is applied in the field of organic compounds with special physical properties of solid state paramagnetism and their synthesis, which can solve problems such as slow progress and achieve the effect of good magnetic function.
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Embodiment 1
[0026] First, in a 250mL four-neck flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 30.5g (0.167mol) of 3-chlorophthalic anhydride and succinic acid (molar ratio is 1: 1), and heat up to 210°C. Start stirring, add potassium acetate (the molar ratio of potassium acetate to 3-chlorophthalic anhydride is 0.2:1), and react at 210°C for 2 hours. Then lower the temperature to 100°C, add hot water and introduce steam. Until the reaction product forms crushed particles, filter, wash the product with hot water, dry, and boil with ethanol to remove resinous impurities. Filter again, wash with ethanol until the eluate is colorless, and dry to obtain 16.0 g of reddish-yellow powder, which is the intermediate for the synthesis of 3-chlorindrone.
[0027] Second, in a 250mL four-necked flask equipped with a thermometer, a reflux condenser and a mechanical stirrer, suspend 16.0g of the intermediate with methanol, raise the temperature to 60°C, and drop the...
Embodiment 2
[0029] First, in a 250mL four-necked flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 30.5g (0.167mol) of 3-chlorophthalic anhydride and succinic acid (molar ratio is 1: 1.5), and heat up to 210°C. Start stirring, add potassium acetate (the molar ratio of potassium acetate to 3-chlorophthalic anhydride is 0.3:1), and react at 210°C for 2 hours. Then lower the temperature to 100°C, add hot water and introduce steam. Until the reaction product forms crushed particles, filter, wash the product with hot water, dry, and boil with ethanol to remove resinous impurities. Filter again, wash with ethanol until the eluate is colorless, and dry to obtain 18.0 g of reddish-yellow powder, which is the intermediate for the synthesis of 3-chlorindrone.
[0030] Second, in a 250mL four-neck flask equipped with a thermometer, a reflux condenser and mechanical stirring, suspend 18.0g of the intermediate with methanol, raise the temperature to 60°C, and quickly...
Embodiment 3
[0032] First, in a 250mL four-neck flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 30.5g (0.167mol) of 3-chlorophthalic anhydride and succinic acid (molar ratio is 1: 2), and heat up to 210°C. Start stirring, add potassium acetate (the molar ratio of potassium acetate to 3-chlorophthalic anhydride is 0.25:1), and react at 210°C for 2 hours. Then lower the temperature to 100°C, add hot water and introduce steam. Until the reaction product forms crushed particles, filter, wash the product with hot water, dry, and boil with ethanol to remove resinous impurities. Then filter, wash with ethanol until the eluate is colorless, and dry to obtain 17.5 g of reddish-yellow powder, which is the intermediate for the synthesis of 3-chlorindrone.
[0033]Second, in a 250mL four-necked flask equipped with a thermometer, a reflux condenser and mechanical stirring, suspend 16.0g of the intermediate with methanol, heat up to 60°C, and drop the sodium methoxid...
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