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Method for preparing high-purity carmustine
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A carmustine, organic solvent technology, applied in the field of medicine, can solve the problem of not giving carmustine and the like
Inactive Publication Date: 2020-03-31
JIANGSU HENGRUI MEDICINE CO LTD
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[0008] However, the existing preparation methods do not provide a method for how to efficiently prepare and obtain high-purity, high-quality carmustine
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Embodiment 1
[0062] Embodiment 1: Preparation of carmustine crude product
[0063]
[0064] Step 1: Add 14.08kg of 2-oxazolidinone and 9.92kg of ethanolamine into the reaction kettle, stir and mix well, heat to 110-120°C for reaction, after the reaction, add 48L of ethanol and 96L of acetone, heat to dissolve, and cool down to 0 Stir and crystallize at -10°C, filter, wash, and dry to obtain 12.22 kg of white solid.
[0065] Step 2: Add the intermediate obtained in step 1) to the reaction kettle, add 29.52 kg of thionylchloride dropwise, stir the reaction, cool down to room temperature after the reaction, add 2.0L of purified water dropwise to quench the reaction, add 24L of ethanol, and activate the carbon to reflux Decolorize, filter, wash the filtrate into 60L water, spin filter, reflux the filter cake with 120L acetone to dissolve, lower the temperature to 0-10°C, stir and crystallize, spin filter, wash, and dry to obtain 5.02kg of white solid. Step 3:
[0066] Add the intermediat...
Embodiment 2
[0068] Dissolve 3.6kg of the solid obtained in Example 1 in a mixed solution of 24L (18.94kg) of ethanol and 12L of purified water, slowly cool down to -15°C, stir and crystallize, filter, wash, and dry (vacuum 25°C, 20h) to obtain sample 2.04 kg, detected by HPLC, the purity is 99.8%, colorless / white powder, the amount of residual solvent ethanol is about 0.05%.
Embodiment 3
[0070] Take 5 g of the solid obtained in Example 1, dissolve it in 50 ml of ethanol, heat to dissolve, slowly cool down to -15 ° C, stir and crystallize, filter, wash, and dry (vacuum 25 ° C, 20 h) to obtain 1.8 g of the sample, which is detected by HPLC and has a purity of 98.4 %, yield 36%, light yellow-green solid, and the amount of residual solvent ethanol is about 0.08%.
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Abstract
The invention provides a method for preparing high-purity carmustine. Specifically, the preparation method comprises a step of recrystallizing a crude carmustine product with an organic solvent, wherein the organic solvent is a mixed solvent of an alcoholsolvent and water, and the alcoholsolvent is preferably at least one selected from the group consisting of methanol, ethanol and isopropanol. The method can be used for preparing high-purity carmustine.
Description
technical field [0001] The invention belongs to the technical field of medicine and relates to a method for preparing high-purity carmustine. Background technique [0002] Carmustine (carmustine), the structure is as follows, the product is a broad-spectrum anticancer drug. It has good curative effect on Hodgkin's disease and acute leukemia, and also has certain curative effect on breast cancer, lungcancer, brain tumor and bone metastasis of cancer. [0003] [0004] As early as 1963, Journal of Medicinal Chemistry 1963, 6, 669-681 has disclosed the preparation method of 1,3-bis(2-chloroethyl)-1-nitrosourea (ie, carmustine). [0005] US2288178 and J.Med.Chem., 1979, 22(10), pp 1193-1198 also respectively describe a new preparation method of carmustine. [0006] Recently, WO2017154019 has described a kind of technology of carmustine again, namely, utilize 2-chloroethylamine or its salt and carbonyldiimidazole (CDI) to prepare 1,3-bis(α-chloroethyl) urea, then In nitros...
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