- Preparation method of
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The invention provides a preparation method of and an intermediate thereof. The preparation method comprises the following steps: carrying out chlorination reaction on the compound of the formula N - 7 N - 3 with a chlorination reagent, then carrying out a fluorine reaction with the fluorine-containing reagent, and reacting the compound as follows. Of these, the chlorinating agent is selected from the sulfonyl chlorides of aromatic hydrocarbons, in particular benzenesulfonyl chloride. At least one of p-toluenesulfonyl chloride and p-chlorobenzoyl chloride, wherein the fluorine-containing agent is hydrofluoric acid. The preparation method is efficient, green and environment-friendly, shortens the production cycle, reduces a large amount of wastewater, improves the yield, reduces the production cost, realizes clean production, HPLC content of the product is less than 99.0%, and the yield reaches 0.10% 100% or more.
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Paragraph 0029; 0048-0053
(2021/10/13)
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- Preparation process of halcinonide intermediate
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The invention provides a prepration process of a halcinonide intermediate. The preparation process comprises the steps: taking a hydrofluoric acid-acetone mixed solvent as a solvent, slowly adding an intermediate N-3 at subzero 40 DEG C to subzero 30 DEG C, carrying out reaction for 4 to 8 hours after material feeding is completed, enabling the temperature to return to subzero 5 DEG C to 0 DEG C, continuously carrying out reaction for 10 to 30 min, slowly adding reaction fluid into a potassium carbonate solution after the reaction is completed, adjusting the PH value to 7.0 to 7.5, filtering and discharging a product, and drying the product to obtain the halcinonide intermediate with the structure as shown in formula N-5. According to the preparation process, a one-pot method is adopted for production, so that the production steps are effectively simplified, and the production period is shortened; the preparation process is more environment-friendly.
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Paragraph 0008; 0009
(2017/07/19)
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