Preparation method of vitamin D2 derivative
A technology of derivatives and vitamins, applied in the field of preparation of vitamin D2 derivatives, can solve the problem of low yield
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example 1
[0049] (1), the amide phosphorus salt compound represented by formula (IV-1) (reference Tetrahedron 1992, 48, 5151-5162) 1.10 g (2 mmol) was added to 10 mL of ether, replaced with nitrogen, started stirring, controlled the temperature at -20°C, and slowly added n-hexane solution of n-butyllithium with a molar concentration of 2.5M 1.6 mL, the solution turned red, after the dropwise addition was completed, the temperature was raised to room temperature, and the reaction was stirred for 2 hours. Then the reaction solution was cooled to -20°C, and then slowly added 0.89 g (2 mmol) of aldehyde represented by formula (III-1) (prepared with reference to US20120130133), the red color of the solution disappeared, and the reaction was stirred at constant temperature for 2 hours, then heated to room temperature and stirred for 5 hours , add 10 g of dilute hydrochloric acid with a weight concentration of 5% to quench the reaction, separate the organic phase, extract the aqueous phase wi...
example 2
[0053] (1), the amide phosphorus salt compound represented by formula (IV-1) (reference Tetrahedron 1992, 48, 5151-5162) 1.10 g (2 mmol) was added to 10 mL of ether, replaced with nitrogen, started stirring, controlled the temperature at -20°C, and slowly added a n-hexane solution of methyllithium with a molar concentration of 2.5M 1.6 mL, the solution turned red, after the dropwise addition was completed, the temperature was raised to room temperature, and the reaction was stirred for 2 hours. Then the reaction solution was cooled to -20°C, and then slowly added 0.89 g (2 mmol) of aldehyde represented by formula (III-1) (prepared with reference to US20120130133), the red color of the solution disappeared, and the reaction was stirred at constant temperature for 2 hours, then heated to room temperature and stirred for 5 hours , add 10 g of dilute hydrochloric acid with a weight concentration of 5% to quench the reaction, separate the organic phase, extract the aqueous phase w...
example 3
[0057] (1), the amide phosphorus salt compound represented by formula (IV-1) (reference Tetrahedron 1992, 48, 5151-5162 preparation) 1.10 g (2 mmol) was added to 10 mL tetrahydrofuran, nitrogen replacement, stirring was started, the temperature was controlled at -20°C, and n-hexane solution of n-butyllithium with a molar concentration of 2.5M was slowly added 1.6 mL, the solution turned red, after the dropwise addition was completed, the temperature was raised to room temperature, and the reaction was stirred for 2 hours. Then the reaction solution was cooled to -20°C, and then slowly added 0.89 g (2 mmol) of aldehyde represented by formula (III-1) (prepared with reference to US20120130133), the red color of the solution disappeared, and the reaction was stirred at constant temperature for 2 hours, then heated to room temperature and stirred for 5 hours , add 10 g of dilute hydrochloric acid with a weight concentration of 5% to quench the reaction, separate the organic phase,...
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