Amisulpride impurity and preparation method thereof

A technology for amisulpride and impurities, which is applied in the field of amisulpride impurities and its preparation, can solve the problems that the synthesis method has no literature reports, etc., and achieve the effects of simple operation, short reaction route and mild reaction conditions

Active Publication Date: 2020-06-12
NANJING HEALTHNICE MEDICAL TECH +2
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Problems solved by technology

Compound II is a new compound structure, and its syn...
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Abstract

The invention belongs to the technical field of medicinal chemistry, in particular to an amisulpride impurity and a preparation method thereof. The preparation method comprises the following steps: inthe co-existence of a condensing agent and an activating agent, a compound I is subjected to a self-condensation reaction at the temperature of 10-70 DEG C, and a compound crude product shown as a formula (II) is prepared, wherein the molar ratio of the compound I to the condensing agent is 1: (0.4-0.7), the molar ratio of the compound I to the activating agent is 1: (0.4-0.7), and the specific is shown as follows.

Application Domain

Organic chemistryOrganic compound preparation +1

Technology Topic

Combinatorial chemistryPharmaceutical Substances +4

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  • Amisulpride impurity and preparation method thereof
  • Amisulpride impurity and preparation method thereof
  • Amisulpride impurity and preparation method thereof

Examples

  • Experimental program(1)
  • Comparison scheme(3)

Example Embodiment

[0034] Example 1
[0035] Add 4-amino-5-(ethylsulfonyl)-2-methoxybenzoic acid (Compound I) (8.0g, 30.84mmol) and N,N-dimethylformamide (30ml) to a 50mL three-necked flask , Stir to dissolve, add 4-dimethylaminopyridine (1.88g, 15.4mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.96g, 15.4mmol) in sequence , The temperature was raised to 25-40°C, the reaction was stirred for 12h, water (300ml) was added, and the mixture was stirred for 1h. A solid precipitated out and filtered to obtain a light yellow solid. The pale yellow solid was stirred and dissolved with ethyl acetate (300ml), washed with water (100ml×2), washed with 1mol/L hydrochloric acid (100ml), washed with saturated sodium bicarbonate aqueous solution (100ml), washed with saturated brine (100ml) Wash, dry with anhydrous sodium sulfate, filter, and concentrate under reduced pressure at 40°C to obtain 10g of crude product. Add ethyl acetate (100ml) to the crude product. Heat to 60~70℃ and stir for 2~3h. Cool to 5~10℃ and stir for 2~3h. , A large amount of solids precipitated, filtered and dried to obtain 5.60 g with a yield of 72.52%. 1 H NMR (500MHz, DMSO-d6) δ: 8.11 (s, 2H), 6.93 (s, 4H), 6.53 (s, 2H), 3.81 (s, 6H), 3.22 (q, J = 7.25 Hz, 4H) , 1.15(t, J=7.3Hz, 6H); TOF MS ES(-)(m/z): 499.10[MH] - ); TOF MS ES(+)(m/z): 523.10[M+Na] + ).

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