Preparation method and analysis and detection method of compound
A compound, the technology of thionyl chloride, is applied in the field of preparation of the pharmaceutical intermediate compound 4-chloromethyl cinnamate methyl ester, which can solve the problems that the preparation method needs to be improved, and achieve mild conditions, high yield and simple method Effect
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Embodiment 4
[0059] Example 4 is a comparative example. In this example, the inventor adjusted the mass volume ratio of the compound shown in formula 1 to sulfuric acid and methanol to be 1:0.2:5. In terms of technical effect, the product yield obtained in this example It is lower than the product yield when the mass volume ratio of the compound represented by formula 1 to sulfuric acid and methanol is 1:0.1:(7.5-20) (g / v / v).
[0060] The compound shown in formula 1 (2g, 11.22mmol) was added to methanol (10ml) and stirred to dissolve, then sulfuric acid (0.2ml) was added, the temperature was raised to 70°C and the reaction was stirred overnight. After the completion of the reaction was detected by TLC, methanol was evaporated to dryness, and then used The pH of the reaction solution was adjusted to neutral with saturated sodium bicarbonate solution, and then extracted with ethyl acetate three times (50ml×3), and then the organic phase was concentrated under reduced pressure and evaporated t...
Embodiment 8
[0070] Example 8 is a comparative example. In this example, the inventor adjusted the molar ratio of the compound shown in formula 2 to thionyl chloride to 1:4.5, and the reaction conditions of the compound shown in formula 2 and thionyl chloride. It is adjusted to keep stirring at 65°C for 2h. In terms of technical effect, the product yield and product purity obtained in this example are lower than those in which the molar ratio of the compound shown in formula 2 and thionyl chloride is 1:(1.2~3) Product yield and purity.
[0071] The compound shown in formula 2 (2.50 g, 13 mmol) was added to dichloromethane (40 mL) to dissolve, and thionyl chloride (6.96 g, 58.5 mmol) was slowly added under stirring, and the reaction was kept at 65 °C for 2 h. TLC detected that the reaction was complete. Then, the dichloromethane and thionyl chloride were removed by concentration under reduced pressure, and then the pH of the obtained crude product was adjusted to neutrality with saturated s...
Embodiment 9
[0072] Embodiment 9 is to the detection of compound shown in formula I
[0073] The method is high performance liquid chromatography, and the high performance liquid chromatography analysis conditions are:
[0074] High performance liquid chromatograph equipped with UV detector, chromatographic column is octadecylsilane bonded silica gel as filler (C18, 4.6×250mm, 5μm) or equivalent chromatographic column, detection wavelength: 289nm, flow rate: 1.0ml / min, column temperature: 30 °C, injection volume: 20 μl. The mobile phase composition is: mobile phase A is 0.1% phosphoric acid aqueous solution; mobile phase B is methanol.
[0075] The conditions for carrying out the elution gradient are as follows:
[0076]
[0077] The chromatogram contains the peak of the compound represented by the formula I, and the retention time of the compound represented by the formula I is about 12.878min, as shown in the appendix. image 3 shown.
[0078] Results: Calculated by the area norm...
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