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Crystal form of solvate of 7β, 10β-dimethoxydocetaxel and preparation method thereof

A technology of docetaxel and dimethoxy, which is applied in the crystal form C of methyl tert-butyl ether compound and its preparation field, can solve the problems that the crystal form and preparation method have not been reported in the literature, and achieve good reproducibility, The effect of clear process and simple operation

Active Publication Date: 2016-01-13
QILU PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although various modified compounds based on 7β, 10β-dimethoxydocetaxel are increasingly disclosed, 7β, 10β-dimethoxydocetaxel isopropyl acetate and methyl tert-butyl Ether compounds and their crystal forms and preparation methods have not been reported in the literature

Method used

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  • Crystal form of solvate of 7β, 10β-dimethoxydocetaxel and preparation method thereof
  • Crystal form of solvate of 7β, 10β-dimethoxydocetaxel and preparation method thereof
  • Crystal form of solvate of 7β, 10β-dimethoxydocetaxel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 17

[0052] Example 17 Preparation of crystalline form B of 17β, 10β-dimethoxydocetaxel acetate isopropyl acetate

[0053] Add 1.0g of 7β, 10β-dimethoxydocetaxel to 25ml of isopropyl acetate, heat at 90°C until the reaction liquid dissolves, stir for 10 minutes, cool down to 20-30°C and continue to stir and crystallize for 23 hours. Suction filtration, washing with 10 ml of isopropyl acetate, and vacuum drying at 40°C for 4 hours gave 0.80 g of a white solid with a yield of 72.0% and a purity of 99.3% by HPLC.

[0054] 1 H-NMR (600MHz, CDCl 3 ,δppm): 1.20(d,3H), 1.22(d,3H), 1.23(d,3H), 1.25(d,3H), 1.36(s,9H), 1.71(s,3H), 1.79(mt, 1H),1.87(s,3H),2.02(s,3H)2.25-2.32(mt,2H),2.36(s,3H),2.69(mt,1H),3.30(s,3H),3.41(mt, 1H),3.45(s,3H),3.82(d,1H),3.85(dd,1H),4.17(d,1H),4.30(d,1H),4.63(s,1H),4.79(s,1H ),4.97(d,1H),5.01(mt,1H),5.27(d,1H),5.41(d,1H),5.63(d,1H),6.20(t,1H),7.31-7.41(mt, 5H), 7.48(t, 2H), 7.60(t, 1H), 8.09(d, 2H).

[0055] The crystal form B of the isopropyl acetate of 7β,...

Embodiment 27

[0062] Example 27 Preparation of crystalline form B of β, 10β-dimethoxydocetaxel acetate isopropyl acetate

[0063] Add 1.0g of 7β,10β-dimethoxydocetaxel to 75ml of isopropyl acetate, heat at 100°C until the reaction liquid dissolves, stir for 10 minutes, cool down to 20-30°C and continue to stir and crystallize for 15 hours. Suction filtration, washing with 10 ml of isopropyl acetate, and vacuum drying at 40°C for 4 hours gave 0.77 g of a white solid with a yield of 69.3% and a purity of 99.4% by HPLC.

[0064] According to XRPD, thermogravimetric analysis and differential scanning volume data, the obtained crystal form is the crystal form B of 7β, 10β-dimethoxydocetaxel acetate isopropyl acetate described in the present invention.

Embodiment 37

[0065] Example 37 Preparation of crystalline form B of β, 10β-dimethoxydocetaxel acetate isopropyl acetate

[0066] Add 1.0g of 7β,10β-dimethoxydocetaxel to 40ml of isopropyl acetate, heat at 110°C until the reaction liquid dissolves, stir for 5 minutes, cool down to 20-30°C and continue to stir and crystallize for 20 hours. Suction filtration, washing with 10 ml of isopropyl acetate, and vacuum drying at 40°C for 4 hours gave 0.78 g of a white solid with a yield of 70.2% and a purity of 99.4% by HPLC.

[0067]According to XRPD, thermogravimetric analysis and differential scanning volume data, the obtained crystal form is the crystal form B of 7β, 10β-dimethoxydocetaxel acetate isopropyl acetate described in the present invention.

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Abstract

The invention belongs to the field of pharmaceutical and chemical industry and relates to a crystal form B of isopropyl acetate esters of 7 beta,10 beta-dimethoxy docetaxel, a crystal form C of methyl tert-butyl ethers of 7 beta,10 beta-dimethoxy docetaxel and preparation methods for the crystal forms. The crystal form B of isopropyl acetate esters of 7 beta,10 beta-dimethoxy docetaxel and the crystal form C of methyl tert-butyl ethers of 7 beta,10 beta-dimethoxy docetaxel are high in stability, high in solubility and high in solution velocity in ethanol, and can be more suitable for industrial production of 7 beta,10 beta-dimethoxy docetaxel preparations.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a crystal form B of isopropyl acetate of 7β, 10β-dimethoxydocetaxel and methyl tert-butyl ether of 7β, 10β-dimethoxydocetaxel Crystal form C of compound and preparation method thereof; said 7β, 10β-dimethoxydocetaxel isopropyl acetate crystal form B and 7β, 10β-dimethoxydocetaxel methyl tert-butyl ether The crystal form C of the compound has good stability, and has good solubility and dissolution rate in ethanol, so it is more suitable for the industrial production of 7β, 10β-dimethoxydocetaxel preparations. Background technique [0002] Prostate cancer is the most common malignant tumor of the male reproductive system, occupying the second place in male tumors, and there are more than 900,000 new cases and nearly 260,000 deaths worldwide every year. The incidence of prostate cancer increases with age. The current drugs for the treatment of prostate cancer mainly in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/14A61P35/00
CPCC07D305/14
Inventor 李书彬林栋王新胜杨成喜范传文
Owner QILU PHARMA CO LTD