A kind of benzimidazole derivative and its preparation method and application
A technology of benzimidazole and derivatives, applied in the field of medicine, achieves the effects of both prevention and treatment, alleviation of symptoms, and convenience in taking
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[0061] The present invention also provides a preparation method of the compound of general formula I, adding the compound of formula II and the compound of formula III into the solvent at a molar ratio of 1:1.05, adding the basic catalyst according to the molar ratio of the compound of formula II and the basic catalyst of 1:0.7, and reacting at room temperature After 10 minutes, evaporate to dryness and recrystallize with ethanol to obtain the compound of formula IV. The compound of formula IV and the oxidizing agent are subjected to oxidation reaction at a molar ratio of 1:0.7 for 1 h at a reaction temperature of -10-0° C., and then separated and purified by column chromatography to obtain the compound of formula I. The solvent is selected from dichloromethane, N,N-dimethylformamide, a mixed solvent of dichloromethane and N,N-dimethylformamide; the basic catalyst is selected from sodium hydroxide, potassium hydroxide, ammonia, oxidation Calcium and its aqueous solution, triet...
example 1
[0066] Example 1: Synthesis of 5-chloro-2-mercapto-1-methylbenzimidazole (a1)
[0067] Put 310mg (2mmol) of 2-amino-4-chloro-N-methylaniline and 804mg (5mmol) of potassium ethyl xanthate into a 10mL microwave tube, add 2mL of DMF, stir to completely dissolve, then put into the microwave, Under the conditions of 160psi, 45w, and 165°C, the reaction was complete in 3 minutes to obtain a red clear solution, which was diluted with 30mL of water, and the pH was adjusted to 3-4 with acetic acid, and a milky white solid was precipitated. It was filtered under reduced pressure to obtain 261 mg of off-white solid, which was recrystallized from ethanol to obtain 197 mg of white flocculent solid with a yield of 50.1%. mp 239.5-241°C; 1 H NMR (400MHz, DMSO-d 6 )δ12.87(s,1H), 7.39(d,J=8.4Hz,1H),7.25(d,J=8.4Hz,1H),7.19(s,1H),3.64(s,3H).
example 2
[0068] Example 2: Synthesis of 5-fluoro-2-mercapto-1-methylbenzimidazole (a2)
[0069] According to the preparation method of a1, 397 mg of white floc was obtained from 2-amino-4-fluoro-N-methylaniline and potassium ethyl xanthate, with a yield of 64.1%. mp 239-240°C. 1 H NMR (400MHz, DMSO-d 6 )δ12.85(s,1H), 7.40–7.36(m,1H),7.13–6.98(m,2H),3.64(s,3H).
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