Preparation method of 2<nd>-crystal form flumioxazin and preparation method of flumioxazin
A technology of profenachlor and 2nd-, which is applied in the field of organic synthesis, can solve problems such as complicated operation, and achieves the effect of simple operation and favorable industrial production.
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[0022] According to a first aspect of the present invention, the present invention provides a 2 nd -The preparation method of crystalline form of fluoriferamic, the method comprising: lowering the temperature of the hot solution in which fluorfen is dissolved at the first temperature to the crystallization temperature for crystallization to obtain 2 nd - crystalline form of flufenazim, wherein the crystallization temperature is 0-10°C, the first temperature is higher than the crystallization temperature, and the solvent of the hot solution is CH 3 COOH.
[0023] In the present invention, CH 3 COOH is preferably provided in the form of acetic acid, for example at a concentration of 95-99% by weight acetic acid, more preferably 97-99% by weight acetic acid, most preferably 99% by weight acetic acid.
[0024] In the present invention, the temperature of the hot solution dissolved in flumechlor propargyl at the first temperature is cooled to the crystallization temperature for c...
Embodiment 1
[0072] Take 10g of 6-amino-7-fluoro-4-propynyl-1,4-benzoxazin-3(4H)-one and 30mL acetic acid (concentration is 99% by weight, the same as below) with a purity of 99% by weight ), 1.05 times the equivalent of 3,4,5,6-tetrahydrophthalic anhydride with a purity of 99.5% by weight were placed in a reaction flask, reacted at 95°C for 3.5 hours, quickly cooled to 0°C with an ice bath, stirred for 2 hours, and filtered , the resulting solid was washed and dried to give 2 nd - The crystalline form of flurafen propargyl.
[0073] will get 2 nd -Crystal form flurafen is carried out X-ray diffraction spectrogram and DSC determination, wherein, figure 1 for 2 nd - the X-ray diffraction spectrum of the crystalline form of flufenamide, the derived data of the X-ray diffraction spectrum is consistent with the data in Table 1 in WO2013187491A; figure 2 for 2 nd -The DSC figure of crystalline form flufenazol, by figure 1 with figure 2 It was shown that the 2-crystal form of flufenazim...
Embodiment 2
[0075] Take 10g of 6-amino-7-fluoro-4-propynyl-1,4-benzoxazin-3(4H)-one with a purity of 99% by weight and 58mL of acetic acid, 1.05 equivalents of 99.5% by weight % of 3,4,5,6-tetrahydrophthalic anhydride was placed in a reaction flask, reacted at 100°C for 4 hours, quickly cooled to 2°C with an ice bath, stirred for 1 hour, filtered, and the obtained solid was washed and dried to obtain 2 nd - The crystalline form of flurafen propargyl.
[0076] will get 2 nd -The X-ray diffraction pattern and DSC determination of the crystalline form of fluramid are carried out, and the X-ray diffraction pattern and the DSC pattern are the same as those in Example 1, indicating that the 2-crystal form of flumechlor is obtained.
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