New preparation method of 10alpha-methoxy-9,10-MMDL
A technology of dihydroergool and methyl dihydroergolate, which is applied in the field of preparation of 10α-methoxy-9,10-dihydroergodol, which can solve the problems of difficult synthesis technology, harsh reaction conditions and poor product quality and other problems, to achieve the effect of reducing process operation and equipment requirements, simple processing, and good product quality
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[0039] Further, in the preparation method of 10α-methoxy-9,10-dihydroergotol, in step S1, the specific steps of the methoxylation reaction of lysergic acid and methanol are:
[0040] S11. Add lysergic acid to the methanol and sulfuric acid mixture and transfer to the photochemical reactor under the dark, control the quenching temperature to 10±5°C, turn on the UV lamp to irradiate the reaction for 6-18 hours, and the light reaction ends; wherein, the ergot The weight ratio of acid to methanol and sulfuric acid mixture is 1:10-50; wherein, the weight ratio of methanol and sulfuric acid mixture in methanol and sulfuric acid mixture is 1.0-10.0:1.0;
[0041] S12. Control the quenching temperature to 10±5°C, and add the reaction solution to purified water added with organic solvent for quenching;
[0042] S13. Control the temperature to 10±5°C, add dropwise alkali solution to adjust the pH to 9.6±0.2, stand to separate the layers, extract the aqueous phase twice with an organic solvent; ...
Embodiment 1
[0056] The specific steps for preparing 10α-methoxy-9,10-dihydroergotol by adopting the new method for preparing 10α-methoxy-9,10-dihydroergotol of the present invention are as follows:
[0057] 1. Steps for preparing intermediates: add 5.0g of lysergic acid to the mixed solution of 100.0g of methanol and 40.0g of sulfuric acid in the dark, and transfer to the photochemical reactor, control the quenching temperature to 10±5℃, and turn on the UV lamp for 10 hours. When the light reaction is over, the quenching temperature is controlled to 10±5°C, and the reaction solution is added to the organic solvent and purified water for quenching. Control the temperature to 10±5°C, add dropwise alkali solution to adjust the pH to 9.4-9.8, stand still for layering, and extract the aqueous phase twice with an organic solvent. The organic phases were combined, dried over anhydrous sodium sulfate, filtered, the filtrate was distilled under reduced pressure to remove the organic solvent, and the ...
Embodiment 2
[0060] The specific steps for preparing 10α-methoxy-9,10-dihydroergotol by using the method for preparing 10α-methoxy-9,10-dihydroergotol of the present invention are as follows:
[0061] 1. Steps for preparing intermediates: add 5.0g of lysergic acid to the mixed solution of 100.0g of methanol and 40.0g of sulfuric acid in the dark, and transfer to the photochemical reactor, control the quenching temperature to 10±5°C, and turn on the UV lamp for 18 hours. When the light reaction is over, the quenching temperature is controlled to 10±5°C, and the reaction solution is added to the organic solvent and purified water for quenching. Control the temperature to 10±5°C, add dropwise alkali solution to adjust the pH to 9.6±0.2, stand still and separate into layers, and extract the aqueous phase twice with an organic solvent. The organic phases were combined, dried over anhydrous sodium sulfate, filtered, the filtrate was distilled under reduced pressure to remove the organic solvent, an...
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