A kind of lithium complex grease and preparation method thereof
A complex lithium-based, grease technology, applied in the field of grease, can solve the problems of polluted land, rivers and lakes, rare, poor biodegradability, etc.
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Embodiment 1
[0056] Synthesis of O-dimethyloxyphosphoryl-N-3,5-bis(tert-butyl)-4-hydroxyphenylpropionyl-L-serine
[0057] (1) L-serine (represented by formula II-a) (100 mmol, 10.5 g), 40 mL of water was added to the reactor in turn, the temperature was lowered to 0°C, the pH was adjusted to 9.0 with sodium hydroxide, and dimethyl phosphite was added. Ester (represented by formula III-a) (130 mmol, 14.3 g) and tetrabutylammonium bromide (1 mmol, 0.32 g) were added dropwise 50 mL of 12% sodium hypochlorite solution with stirring. After 4 hours of reaction, it was extracted twice with ether, the aqueous layer was adjusted to pH=3 with hydrochloric acid, 8 g of sodium chloride was added, extracted twice with ethyl acetate, the organic phases were combined, dried with anhydrous magnesium chloride, and the solvent was distilled off under reduced pressure to obtain no residue color oil. The colorless oil was dissolved in 60 mL of acetonitrile, sonicated at room temperature for 5 hours, and filt...
Embodiment 2
[0064] Synthesis of O-diisopropyloxyphosphoryl-N-3,5-bis(tert-butyl)-4-hydroxyphenylpropionyl-L-serine
[0065] (1) L-serine (represented by formula II-a) (100 mmol, 10.5 g), 40 mL of water was added to the reactor in turn, the temperature was lowered to 0 °C, the pH was adjusted to 9.0 with sodium hydroxide, and diisophosphite was added. Propyl ester (represented by formula III-b) (130 mmol, 21.7 g) and tetrabutylammonium bromide (1 mmol, 0.32 g) were added dropwise 50 mL of 12% sodium hypochlorite solution with stirring. After 4 hours of reaction, it was extracted twice with ether, the aqueous layer was adjusted to pH=3 with hydrochloric acid, 8 g of sodium chloride was added, extracted twice with ethyl acetate, the organic phases were combined, dried with anhydrous magnesium chloride, and the solvent was distilled off under reduced pressure to obtain no residue color oil. The colorless oil was dissolved in 60 mL of acetonitrile, sonicated at room temperature for 5 hours, a...
Embodiment 3
[0072] Synthesis of O-diphenylmethyl oxyphosphoryl-N-3,5-bis(tert-butyl)-4-hydroxyphenylpropionyl-L-serine
[0073] (1) L-serine (represented by formula II-a) (100 mmol, 10.5 g), 40 mL of water was added to the reactor in turn, the temperature was lowered to 0°C, the pH was adjusted to 9.0 with sodium hydroxide, and dibenzyl phosphite was added. Esters (represented by formula III-c) (130 mmol, 34.0 g) and tetrabutylammonium bromide (1 mmol, 0.32 g) were added dropwise with stirring 50 mL of 12% sodium hypochlorite solution. After 4 hours of reaction, it was extracted twice with ether, the aqueous layer was adjusted to pH=3 with hydrochloric acid, 8 g of sodium chloride was added, extracted twice with ethyl acetate, the organic phases were combined, dried with anhydrous magnesium chloride, and the solvent was distilled off under reduced pressure to obtain no residue color oil. The colorless oil was dissolved in 60 mL of acetonitrile, sonicated at room temperature for 5 hours, ...
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