A kind of preparation method of glimepiride intermediate
A technology for intermediates and compounds, applied in the field of API preparation, can solve the problems of impurities Ⅴ and Ⅵ exceeding the standard and exceeding the limit, difficult to remove, and low impurity content.
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Embodiment 1(1
[0047] Example 1 (1.0 molar equivalent of acetic acid)
[0048] Compound IX. 5.0g, 4-(2-aminoethyl)benzenesulfonamide 4.08g, acetic acid 1.22g and isopropanol 50g heated reflux for 8h (4-(2-aminoethyl)benzene sulfonamide remaining amount of 0.74%), cooled 25 °C, filtered, 50 °C dryed to compound I.6.67g, HPLC detection purity of 99.86%, impurity VIII. 0.05%, impurities V. and VI. undetected, yield 93.2%
Embodiment 2(1
[0049] Example 2 (1.0 molar equivalent acetic acid amplification effect)
[0050] The compound IX. 40.0g, 4-(2-aminoethyl)benzenesulfonamide 32.64g, acetic acid 9.8g and isopropanol 160g were heated and refluxed for 8h, cooled at 25 °C, filtered, and dried at 50 °C to give Compound I. 53.65g, yield 93.6%, HPLC detection purity of 99.78%, impurity VIII. 0.06%, impurity V. and VI. undetected.
Embodiment 3(2
[0051] Example 3 (2.0 molar equivalent of acetic acid)
[0052]The compound IX. 10.0g, 4-(2-aminoethyl)benzenesulfonamide 8.16g, glacial acetic acid 4.9g and isopropanol 50g heated reflux for 7h, cooled 25 °C, filtered, 50 °C dried to compound I. 13.18g, yield 92.0%, HPLC method detection purity of 99.71%, impurities VIII. 0.04%, impurities V. and VI. undetected.
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