Dipotassium pyridinepentacarboxylic acid compound and preparation method thereof
A technology of potassium compound and pentaformic acid, which is applied in potassium organic compounds, 1/11 group organic compounds without C-metal bonds, organic chemistry, etc., can solve the problems of poor stability and small buffer capacity, and achieve good stability, The effect of large buffer capacity and good prospects for promotion and application
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Embodiment 1
[0026] Example 1 Add 130 g (1.0 mol) ethyl acetoacetate to the reactor, add catalyst ethylenediamine 0.3 g, add 40% acetaldehyde 55 g (0.5 mol) dropwise within 4 hours under stirring, and continue stirring at room temperature for 48 hours , separated the upper aqueous phase, added an equal volume of ethanol to the lower organic phase, saturated it with ammonia gas, let it stand and sealed for 72 hours, and there were light yellow crystals of 2,4,6-trimethyl-1,4-dihydropyridine- Diethyl 3,5-dicarboxylate was precipitated, filtered with suction, half of the alcohol was evaporated from the filtrate, and a yellow solid 2,4,6-trimethyl-1,4-dihydropyridine-3,5-dihydropyridine was precipitated after cooling. Diethyl diformate, yield 33%.
[0027] In another reactor, 135g of water, 39g of 98% sulfuric acid and 38g of 60% nitric acid were added successively under stirring, heated to slight boiling, and 100g of 2,4,6-trimethyl-1,4-dihydropyridine-3 was added, Diethyl 5-dicarboxylate, c...
Embodiment 2
[0028] Embodiment 2: add 130g (1.0mol) ethyl acetoacetate in reactor, add catalyst diethylamine 0.6g, under stirring, dropwise add 40% acetaldehyde 77g (0.7mol) in 6 hours, continue stirring at room temperature for 60 hours, separated the upper aqueous phase, added an equal volume of ethanol to the lower organic phase, saturated it with ammonia gas, left it still and sealed for 96 hours, and there were light yellow crystals of 2,4,6-trimethyl-1,4-dihydropyridine -Diethyl 3,5-dicarboxylate was precipitated, filtered with suction, half of the alcohol was evaporated from the filtrate, and a yellow solid 2,4,6-trimethyl-1,4-dihydropyridine-3,5 - Diethyl dicarboxylate, yield 57%.
[0029] In another reactor, 135g of water, 39g of 98% sulfuric acid and 38g of 60% nitric acid were added successively under stirring, heated to slight boiling, and 100g of 2,4,6-trimethyl-1,4-dihydropyridine-3 was added, Diethyl 5-dicarboxylate, continue to keep warm and boil for 10min, use 50% liquid c...
example 3
[0030] Example 3 Add 130 g (1.0 mol) of ethyl acetoacetate to the reactor, add 1.2 g of catalyst aniline, add 110 g (1 mol) of 40% acetaldehyde dropwise within 8 hours under stirring, continue stirring at room temperature for 72 hours, and separate the upper layer Add equal volume of ethanol to the aqueous phase and the lower organic phase, saturate with ammonia gas, let it stand and seal for 120 hours, there are light yellow crystals of 2,4,6-trimethyl-1,4-dihydropyridine-3,5- Diethyl dicarboxylate precipitated, suction filtered, half of the alcohol was evaporated from the filtrate, and a yellow solid 2,4,6-trimethyl-1,4-dihydropyridine-3,5-dicarboxylic acid diethyl was precipitated after cooling Esters, 50% yield.
[0031] In another reactor, 135g of water, 39g of 98% sulfuric acid and 38g of 60% nitric acid were added successively under stirring, heated to slight boiling, and 100g of 2,4,6-trimethyl-1,4-dihydropyridine-3 was added, Diethyl 5-dicarboxylate, continue to keep...
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