Preparation method of dabigatran etexilate intermediate
A technology of dabigatran etexilate and intermediates, applied in the field of preparation of dabigatran etexilate intermediates, can solve the problems of slow reaction rate, low yield, difficult purification, etc., and achieve easy operation, high reaction rate and high product quality. The effect of high purity
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Embodiment 1
[0029] Compound 1 (21.2g, 56.12mmol) and dimethyl sulfoxide (77.0ml) were added to the reaction kettle, the temperature was raised to 70°C, 27.0%-32.0% methylamine in ethanol solution (21.0ml) was slowly added dropwise, and stirred for 30min. Ethyl acetate (39.0ml) was added to the reaction solution, washed with water, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated to dryness to obtain compound 2 (20.6g, yield 98.56%). mp86~88℃; 1H-NMR (DMSO-d 6 , 400MHz) δ: 1.11(t, 3H), 2.66(t, 2H), 2.91(t, 3H), 3.96(q, 2H), 4.18(t, 2H), 6.83(d, 1H), 7.08(d , 1H), 7.21 (m, 1H), 7.32 (dd, 1H), 7.69 (m, 1H), 7.93 (d, 1H), 8.36 (d, 1H), 8.43 (dd, 1H). HPLC purity 98.3%.
Embodiment 2
[0031] Add compound 1 (5.0g, 13.24mmol) and N,N-dimethylformamide (18.0ml) into the reaction kettle, raise the temperature to 70°C, and slowly add 27.0%-32.0% methylamine in ethanol solution (5.0ml) dropwise , stirred for 30min. Ethyl acetate (10.0ml) was added to the reaction solution, washed with water, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated to dryness to obtain compound 2 (4.8g, yield 97.36%). mp86~88℃; 1H-NMR (DMSO-d 6 , 400MHz) δ: 1.11(t, 3H), 2.66(t, 2H), 2.91(t, 3H), 3.96(q, 2H), 4.18(t, 2H), 6.83(d, 1H), 7.08(d , 1H), 7.21 (m, 1H), 7.32 (dd, 1H), 7.69 (m, 1H), 7.93 (d, 1H), 8.36 (d, 1H), 8.43 (dd, 1H). HPLC purity 98.9%.
Embodiment 3
[0033] Add compound 1 (5.0g, 13.24mmol) and N,N-dimethylacetamide (18.0ml) into the reaction kettle, raise the temperature to 70°C, and slowly add 27.0%-32.0% methylamine in ethanol solution (5.0ml) dropwise , stirred for 30min. Ethyl acetate (10.0ml) was added to the reaction solution, washed with water, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated to dryness to obtain compound 2 (4.9g, yield 99.39%). mp86~88℃; 1H-NMR (DMSO-d 6 , 400MHz) δ: 1.11(t, 3H), 2.66(t, 2H), 2.91(t, 3H), 3.96(q, 2H), 4.18(t, 2H), 6.83(d, 1H), 7.08(d , 1H), 7.21 (m, 1H), 7.32 (dd, 1H), 7.69 (m, 1H), 7.93 (d, 1H), 8.36 (d, 1H), 8.43 (dd, 1H). HPLC purity 98.0%.
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