Method for preparing 7-dehydrocholesterol
A technology for dehydrocholesterol and cholesterol, applied in the direction of steroids, organic chemistry, etc., can solve the problems of environmental harm, restrict development, and many by-products, and achieve the effects of less side reactions, less equipment corrosion, and simple operation.
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Embodiment 1
[0032] 1) Add 5g of cholesterol to 40ml of acetyl chloride, reflux at 100°C for 8h, and react to form cholesterol acetate. The purity of the cholesterol acetate produced by the reaction determined by the internal standard method was 94%, and the yield was 90%.
[0033] 2) Dissolve 5g of cholesterol acetate in 70ml of cyclohexanone, shake well at room temperature, and heat to 50°C. Take 0.3g of selenium dioxide and add it to the reaction solution in batches, and add it in 30 minutes. React at 80°C for 8h, cool down to room temperature, and then cool with 3°C water to precipitate crystals, filter with suction, and dry in vacuum at 50°C for 6h. The purity of the 7-carbonylcholesterol acetate obtained through detection is 86%, and the yield is 65%.
[0034] 3) Dissolve 5 g of 7-carbonylcholesterol acetate and 8 g of p-toluenesulfonyl hydrazide in 50 ml of absolute ethanol, stir at room temperature and monitor with thin layer chromatography, stop the reaction after 15 hours, and ...
Embodiment 2
[0037] 1) Add 5g of cholesterol to 40ml of benzoyl chloride, reflux at 80°C for 6h, and react to generate cholesterol benzoate. The purity of the cholesterol benzoate generated by the reaction determined by the internal standard method was 96%, and the yield was 93%.
[0038] 2) Dissolve 5g of cholesterol benzoate in 70ml of cyclohexanone, shake well at room temperature, and heat to 50°C. Take 0.5g of potassium permanganate and add to the reaction liquid in batches, and the addition is completed within 30 minutes. React at 50°C for 5h, cool down to room temperature, and then cool with 3°C water to precipitate crystals, filter with suction, and dry in vacuum at 50°C for 6h. The purity of 7-carbonylcholesterol benzoate obtained through detection is 87%, and the yield is 69%.
[0039] The following steps are the same as steps 3, 4, and 5) in Example 1.
Embodiment 3
[0041] In this embodiment, step 2) is different from embodiment 1, and other steps are the same as embodiment 1 step. Step 2) of the present embodiment is:
[0042] 2) Dissolve 5g of cholesterol acetate in 70ml of cyclohexanone, shake well at room temperature, and heat to 50°C. Take 0.2 g of dicobalt trioxide and add it to the reaction solution in batches, and the addition is completed in 30 minutes, and oxygen is continuously introduced. React at 90°C for 6h, cool down to room temperature, and then cool with 3°C water to precipitate crystals, filter with suction, and dry in vacuum at 50°C for 6h. The purity of the 7-carbonylcholesterol acetate obtained through detection is 91%, and the yield is 75%.
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