Preparation method of 7-dehydrocholesterol
A technology for dehydrocholesterol and cholesterol, applied in the direction of steroids, chemical recovery, organic chemistry, etc., can solve the problem of low yield and achieve the effects of increased yield, high active bromine content, and economical use
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Embodiment 1
[0020] 1. A method for preparing 7-dehydrocholesterol, comprising the steps of:
[0021] 1) Esterification reaction
[0022] Cholesterol + Benzoyl Chloride → Cholesterol Benzoate
[0023] Material molar ratio: cholesterol: benzoyl chloride 1:1.5
[0024] The synthesis of cholesteryl benzoate is carried out in two steps, one is the synthesis of benzoyl chloride, and the other is the synthesis of cholesteryl benzoate with benzoyl chloride and cholesterol as raw materials. The specific implementation plan is as follows:
[0025] React freshly steamed thionyl chloride with benzoic acid at room temperature for 1 hour at 50±5°C (the molar ratio of thionyl chloride to benzoic acid is 1.05:1), then raise the temperature to 90°C for 2 hours. Excessive thionyl chloride was distilled off at normal pressure, and then benzoyl chloride was distilled off under reduced pressure as the raw material for the next reaction.
[0026] Dissolve cholesterol in dry benzene, add pyridine [W 胆固醇 (g...
Embodiment 2
[0039] 1. A method for preparing 7-dehydrocholesterol, comprising the steps of:
[0040] 1) Esterification reaction
[0041] Cholesterol + Benzoyl Chloride → Cholesterol Benzoate
[0042] Material molar ratio: cholesterol: benzoyl chloride 1:0.9
[0043] The synthesis of cholesteryl benzoate is carried out in two steps, one is the synthesis of benzoyl chloride, and the other is the synthesis of cholesteryl benzoate with benzoyl chloride and cholesterol as raw materials. The specific implementation plan is as follows:
[0044] React freshly steamed thionyl chloride with benzoic acid at room temperature for 1 hour at 50±5°C (the molar ratio of thionyl chloride to benzoic acid is 1.05:1), then raise the temperature to 90°C for 2 hours. Excessive thionyl chloride was distilled off at normal pressure, and then benzoyl chloride was distilled off under reduced pressure as the raw material for the next reaction.
[0045] Dissolve cholesterol in dry benzene, add pyridine [W 胆固醇 (g...
Embodiment 3
[0057] 1. A method for preparing 7-dehydrocholesterol, comprising the steps of:
[0058] 1) Esterification reaction
[0059] Cholesterol + Benzoyl Chloride → Cholesterol Benzoate
[0060] Material molar ratio: cholesterol: benzoyl chloride 1:1.9
[0061] The synthesis of cholesteryl benzoate is carried out in two steps, one is the synthesis of benzoyl chloride, and the other is the synthesis of cholesteryl benzoate with benzoyl chloride and cholesterol as raw materials. The specific implementation plan is as follows:
[0062] React freshly steamed thionyl chloride with benzoic acid at room temperature for 1 hour at 50±5°C (the molar ratio of thionyl chloride to benzoic acid is 1.05:1), then raise the temperature to 90°C for 2 hours. Excessive thionyl chloride was distilled off at normal pressure, and then benzoyl chloride was distilled off under reduced pressure as the raw material for the next reaction.
[0063] Dissolve cholesterol in dry benzene, add pyridine [W 胆固醇 (g...
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