Preparation process of voglibose impurity N-methyl-thymolamine
A technology based on methylenzyme olamine and voglibose, which is applied in the field of drug synthesis, can solve the problems of no published patents or literature reports, and achieve the effects of convenient operation, environmental protection, and simple post-processing
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Embodiment 1
[0024] Add 1.55g (0.008mol) Jinggang enzyme olamine into a 100ml single-necked flask, then add 50ml of anhydrous methanol, then add 1.21g (0.0088mol) of anhydrous potassium carbonate, stir well and add 1.36g (0.0096mol) of iodine dropwise methane, and the reaction was stirred overnight at room temperature. The solid was filtered out, and the anhydrous methanol was concentrated under reduced pressure to obtain 1.53 g of crude N-methyl olamine, with a content of 82.34% and a yield of 75.88%.
Embodiment 2
[0026] In a 100ml single-necked flask, add 1.93g (0.01mol) of olamine, then add 50ml of DMF, then add 1.79g (0.013mol) of anhydrous potassium carbonate, stir evenly and add dropwise 1.98g (0.014mol) of methyl iodide, The reaction was stirred overnight at room temperature. The solid was filtered out, and the DMF was concentrated under reduced pressure to obtain 1.95 g of a crude product of N-methylwellanase olamine with a content of 93.21% and a yield of 87.64%. The obtained crude product was purified to obtain 1.55 g of pure N-methyl olamine, with a content of 99.88%.
[0027] The structure confirmation spectrogram of this embodiment is shown in the appendix Figure 1~6 .
Embodiment 3
[0029] In a 100ml single-necked flask, add 2.32g (0.012mol) olamine, then add 60ml acetonitrile, then add 2.48g (0.018mol) anhydrous potassium carbonate, stir and add dropwise 2.71g (0.0192mol) methyl iodide, The reaction was stirred overnight at room temperature. The solid was filtered out, and the acetonitrile was concentrated under reduced pressure to obtain 2.06 g of a crude product of N-methyl olamine, with a content of 88.22% and a yield of 73.25%.
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