Method for synthesizing VK2 through one-step method
A step-by-step and drop-dropping technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of quinones, etc., can solve the problems of low purity, flammable and explosive, low purity of VK2, etc., and shorten the reaction time and price. Inexpensive, cost-reducing effect
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Embodiment 1
[0027] Add 1g (5.8mmol) menadione to 20ml tetrahydrofuran, then add 2.2g cuprous iodide (11.6mmol), lower the temperature to -78 degrees Celsius under nitrogen protection, then add 5.8ml (11.6mmol) LDA dropwise, and control the temperature After reacting at -78°C for 1 hour, 3 g (8.5 mmol) of geranylgeranyl bromide was added dropwise, then reacted naturally at -78°C for 1 hour, and detected by HPLC. Sampling and sending to liquid phase detection, such as figure 1 As shown, there is a peak content of VK2 of about 34.2%. After the final reaction solution was raised to room temperature, the reaction solution was poured into saturated ammonium chloride aqueous solution to wash, extracted with ethyl acetate, backwashed with saturated brine, dried and then spin-dried, separated and purified by silica gel column, and the eluent was ethyl acetate Ester: Petroleum ether=1:10, v / v, about 300 mg of product can be obtained by removing the solvent, the total yield is 12%, and the liquid p...
Embodiment 2
[0029] Add 10g (58mmol) menadione to 200ml tetrahydrofuran, then add 22g cuprous iodide (116mmol), lower the temperature to -78°C under nitrogen protection, then add 58ml (116mmol) LDA dropwise, and control the temperature at -78°C for reaction 1 Hours later, 30g (85mmol) geranylgeranyl bromide was added dropwise, and then reacted naturally at -78 degrees Celsius for 1 hour. After the final reaction solution was warmed up to room temperature, the reaction solution was poured into saturated ammonium chloride aqueous solution for washing, ethyl acetate Ester extraction, backwashing with saturated brine, drying, spin-drying, separation and purification through a silica gel column, the eluent is ethyl acetate:petroleum ether=1:10, v / v. About 3.1 g of product were obtained.
Embodiment 3
[0031] Add 15g (87mmol) menadione to 250ml tetrahydrofuran, then add 33g cuprous iodide (174mmol), lower the temperature to -78°C under nitrogen protection, then add 87ml (174mmol) LDA dropwise, and control the temperature at -78°C for reaction 1 Hours later, 45g (127.5mmol) geranylgeranyl bromide was added dropwise, and then reacted naturally at -78 degrees Celsius for 1 hour. After the final reaction solution was warmed up to room temperature, the reaction solution was poured into saturated aqueous ammonium chloride solution for washing, acetic acid Extracted with ethyl ester, backwashed with saturated brine and dried, then spin-dried, separated and purified by silica gel column, the eluent was ethyl acetate:petroleum ether=1:10, v / v, and about 4.5 g of the product was obtained.
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