Method for separating 24-dehydrogenation cholesterol and cholesterol
A technology for dehydrocholesterol and cholesterol, applied in the preparation of steroids, chemical instruments and methods, steroids, etc., can solve the problems of low content and yield, cumbersome process, long production cycle, etc. Good separation effect and stable operation
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Embodiment 1
[0019] The mixture of 24-dehydrocholesterol and cholesterol (24-dehydrocholesterol / cholesterol=13.64%, mass ratio) is dissolved in petroleum ether with a boiling range of 60 to 90°C, and the total concentration of 24-dehydrocholesterol and cholesterol is 0.9 g / L of raw material solution. The mixture of methanol and sulfolane with a percentage of sulfolane accounting for 70% of the total volume is used as the extractant, petroleum ether with a boiling range of 60-90° C. is used as the detergent, and the flow ratio of the extractant, detergent, and raw material solution is 6: 4.5:1.5, carry out fractional distillation and extraction at 50°C, collect the extract and raffinate, and concentrate in vacuo to obtain 24-dehydrocholesterol with a purity of 93.83%, a yield of 70.0%, and cholesterol with a purity of 97.86%. The yield was 95.0%.
Embodiment 2
[0021] The raw materials (24-dehydrocholesterol / cholesterol=12.98%, mass ratio) are dissolved in petroleum ether with a boiling range of 60-90° C. to prepare a raw material solution with a total concentration of 24-dehydrocholesterol and cholesterol of 1.8 g / L. The mixture of methanol and sulfolane with a percentage of sulfolane accounting for 70% of the total volume is used as the extractant, petroleum ether with a boiling range of 60-90° C. is used as the detergent, and the flow ratio of the extractant, detergent, and raw material solution is 6: 4.5:0.3, carry out fractional distillation and extraction at 50°C, collect the extract and raffinate, and concentrate in vacuo to obtain 24-dehydrocholesterol with a purity of 96.64%. The yield is 80.0%, and the purity is 98.29%. The yield was 98.5%.
Embodiment 3
[0023] The raw material (24-dehydrocholesterol / cholesterol=13.64%, mass ratio) was dissolved in octane to prepare a raw material solution with a total concentration of 24-dehydrocholesterol and cholesterol of 1.8 g / L. With the mixture of methanol and sulfolane with sulfolane accounting for 50% of the total volume as the extractant, octane as the detergent, the flow ratio of the extractant, detergent, and raw material liquid is 6:3.5:1.5, at 40 ° C Fractional distillation and extraction were carried out, the extract and raffinate were collected, and concentrated in vacuo to obtain 24-dehydrocholesterol with a purity of 85.56%, with a yield of 85.0%, and cholesterol with a purity of 92.10%, with a yield of 99.5%.
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