Synthetic method for aliphatic alpha-calcium picrolonate
A synthetic method and technology of calcium ketoacids, which are applied in the field of synthesis of aliphatic α-ketoacid calcium, and can solve problems such as unsynthesized aliphatic α-ketoacids
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Embodiment 1
[0060] Embodiment 1, the synthesis of calcium α-ketoisocaproate
[0061] (1) Synthesis of isobutylene hydantoin intermediate
[0062] Take 10g hydantoin (0.1mol) and 8g sodium bicarbonate (0.08mol) into a three-necked flask, add water to mix and stir, raise the temperature to 70-80°C, add 9.3g (0.13mol) of isobutyraldehyde, reflux for 8 hours, and cool After reaching room temperature, 50% sulfuric acid was added to adjust the pH value, a large amount of solid precipitated, filtered and washed with water, and the dried white solid isobutylidene hydantoin was 12.4g, the yield was 81%, and the melting point was 120-122°C. Elemental analysis is qualified.
[0063] (2) Synthesis of calcium α-ketoisocaproate
[0064] Put 15.4 g (0.1 mol) of isobutylene hydantoin and 100 ml of 20% sodium hydroxide solution in a three-necked flask, stir and reflux for 2 hours, adjust the pH value with 50% sulfuric acid, evaporate the water to dryness under reduced pressure, and add methanol Extract...
Embodiment 2
[0065] Embodiment 2, the synthesis of α-ketoisovalerate calcium
[0066] (1) Synthesis of isopropylidene hydantoin intermediate
[0067] Add 10g (0.1mol) of hydantoin, add 12ml of water, stir and heat to 60°C, add 7.54g (0.13mol) of acetone, add 4.8g (0.08mol) of ethanolamine dropwise in 30 minutes, and stir and react at 70°C for 6 hours after dropping, the reaction is completed After cooling, the pH was adjusted to 4 with concentrated HCl to precipitate a solid, which was filtered, washed and dried with 10 ml of water to obtain 13.3 g, with a yield of 95%. The melting point is 279°C, and the elemental analysis is qualified.
[0068] (2) Synthesis of α-ketoisovalerate calcium
[0069] Take 14 g (0.1 mol) of mesitylidene hydantoin intermediate and 100 g of 20% (mass ratio) NaOH solution, heat and reflux at 110 degrees Celsius for 2 hours, cool after the reaction and adjust the pH to 5 with concentrated HCl, cool and filter to remove the solid, and the filtrate Concentrate to...
Embodiment 3
[0070] Embodiment 3, the synthesis of α-keto-β-methylvalerate calcium
[0071] (1) Synthesis of isobutyl hydantoin intermediate
[0072] Add 10g (0.1mol) of hydantoin, add 12ml of water, stir and heat to 60°C, add 9.37g (0.13mol) of butanone, dropwise add 4.8g (0.08mol) of ethanolamine, and stir and react at 80°C for 4 hours. Concentrated HCl was adjusted to PH=4, and a solid precipitated out, which was filtered, washed with distilled water and dried to obtain 9.4 g with a yield of 61%, and the elemental analysis was qualified.
[0073] (2) Synthesis of α-keto-β-methylpentanoic acid calcium salt
[0074] Take 15.4g (0.1mol) of the intermediate and 100g of 20% (mass ratio) NaOH solution, heat to reflux for 2 hours, 110 degrees Celsius, adjust the pH to 5 with concentrated HCl after the reaction, cool and filter to remove the solid, and concentrate the filtrate to dryness under reduced pressure , add 150ml of anhydrous methanol and heat to reflux for 1 hour, filter while it is...
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