Synthesis of vitamin D2 derivatives
A vitamin and synthesis method technology, applied in the field of synthesis of vitamin D2 derivatives, can solve the problems of heavy metal residues, low oxidation activity of manganese dioxide, etc., and achieve the effects of mild conditions, improved atom utilization, and environmental friendliness
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Embodiment 1
[0024] Example 1: DMP (1.315 g, 3.1 mmol) in dichloromethane (5 mL) was added dropwise to compound 1 (2 g, 3.1 mmol) in dichloromethane (20 mL) under argon protection at room temperature After the dropwise addition was completed, stirring was continued at room temperature for 2 hours. After the reaction was complete, 20 mL of saturated aqueous sodium bicarbonate was added, stirred at room temperature for 30 minutes, and filtered under reduced pressure. The filtrate was extracted three times with dichloromethane, the organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate for 2 hours. Suction filtration under reduced pressure, the filtrate was concentrated under reduced pressure, and column chromatography gave compound 2 (1.75 g, 88%) as a white solid.
Embodiment 2
[0025] Example 2: DMP (1.45 g, 3.41 mmol) in dichloromethane (5 mL) was added dropwise to compound 1 (2 g, 3.1 mmol) in dichloromethane (20 mL) under argon protection at room temperature After the dropwise addition was completed, stirring was continued at room temperature for 2 hours. After the reaction was complete, 20 mL of saturated aqueous sodium bicarbonate was added, stirred at room temperature for 30 minutes, and filtered under reduced pressure. The filtrate was extracted three times with dichloromethane, the organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate for 2 hours. Suction filtration under reduced pressure, the filtrate was concentrated under reduced pressure, and column chromatography gave compound 2 (1.83 g, 92%) as a white solid.
Embodiment 3
[0026] Example 3: DMP (1.45 g, 3.41 mmol) in dichloromethane (5 mL) was added dropwise to compound 1 (2 g, 3.1 mmol) in dichloromethane (20 mL) under argon protection at room temperature , After the dropwise addition was completed, the mixture was stirred under reflux at 40° C. for 2 hours. After the reaction was complete, 20 mL of saturated aqueous sodium bicarbonate was added, stirred at room temperature for 30 minutes, and filtered under reduced pressure. The filtrate was extracted three times with dichloromethane, the organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate for 2 hours. Suction filtration under reduced pressure, the filtrate was concentrated under reduced pressure, and column chromatography gave compound 2 (1.65 g, 83%) as a white solid.
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