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A kind of crystallization method of pharmaceutical intermediate

An intermediate and crystallization technology, applied in the field of chemistry, can solve problems such as the crystallization method of compound I that has not been reported in the literature

Active Publication Date: 2018-06-12
江苏阿尔法集团福瑞药业(宿迁)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, no literature has reported the crystallization method of compound I

Method used

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  • A kind of crystallization method of pharmaceutical intermediate
  • A kind of crystallization method of pharmaceutical intermediate
  • A kind of crystallization method of pharmaceutical intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Dissolution: Take 13.23g of the crude compound I (R=Cl), add 50ml of ethyl acetate, add 0.5g of activated carbon, heat up to 80°C and stir for 30min, then suction filter while it is hot, and collect the filtrate;

[0042] Crystallization: the filtrate is slowly cooled to 55°C, and 200ml of petroleum ether is added dropwise to it to form a small amount of crystals;

[0043] Crystal growth: in the first stage, stir in the solution in which crystals appear at a stirring speed of 190rpm, so that the temperature of the solution drops to 30°C, and then keep it warm for 3 hours; in the second stage, stir the solution again at a stirring speed of 80rpm , and in the process of stirring, the temperature of the solution was reduced to 0°C, and then kept for 3 hours; in the third stage, the solution was stirred again at a speed of 50rpm, so that the temperature of the solution rose to 30°C, and stood for 12 Hours, crystallization, and suction filtration; wherein, the cooling rate o...

Embodiment 2

[0047] Dissolution: Take 13.23g of crude compound I (R=Br), add 45ml of ethyl acetate, add 0.6g of activated carbon, heat up to 75°C and stir for 30min, then suction filter while it is hot, and collect the filtrate;

[0048] Crystallization: Slowly cool the filtrate to 50°C, add 190ml of petroleum ether dropwise to it, and a small amount of crystals appear;

[0049] Crystal growth: in the first stage, stir in the solution in which crystals appear at a stirring speed of 200rpm, so that the temperature of the solution drops to 40°C, and then keep warm for 2.5 hours; in the second stage, stir the solution again at a stirring speed of 80rpm , and in the process of stirring, the temperature of the solution was reduced to -10°C, and then kept for 3 hours; in the third stage, the solution was stirred again at a speed of 50 rpm, so that the temperature of the solution rose to 30°C, and stood 12 hours, crystallization, and suction filtration; wherein, the cooling rate of the first stag...

Embodiment 3

[0053] Dissolution: Take 13.23g of crude compound I (R=Cl), add 40ml of methanol, add 0.3g of activated carbon, heat up to 80°C and stir for 30min, then suction filter while it is hot, and collect the filtrate;

[0054] Crystallization: the filtrate is slowly cooled to 55°C, and 160ml of n-heptane is added dropwise to it to produce a small amount of crystals;

[0055]Crystal growth: in the first stage, stir in the solution in which crystals appear at a stirring speed of 200rpm, so that the temperature of the solution drops to 40°C, and then keep warm for 2.5 hours; in the second stage, stir the solution again at a stirring speed of 90rpm , and in the process of stirring, the temperature of the solution was reduced to 10°C, and then kept for 3.5 hours; in the third stage, the solution was stirred again at a speed of 60rpm, so that the temperature of the solution rose to 30°C, and stood for 15 Hours, crystallization, and suction filtration; wherein, the cooling rate of the first...

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Abstract

The invention discloses a crystallization method of a drug intermediate, and relates to the chemical field. The method comprises that a crude product is subjected to the steps of dissolving, crystallization, crystal growing and drying, and a compound I is extracted from a crude product solution. The method is simple to operate, higher in yield and purity, low in cost of used raw materials, and suitable for industrialized production; in a formula I, an R group is Cl and Br.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a crystallization method of a drug intermediate. Background technique [0002] Pharmaceutical intermediate compound I is a 5-halogenated tetrahydrofuran compound, and is an important pharmaceutical intermediate for preparing compound III. [0003] [0004] Wherein, the R group is Cl or Br. [0005] Through experiments and literature reports, it is known that the reduction of compound IV through red aluminum and halogenation reaction has obtained a group of mixtures, in which only the configuration of compound I is required for the next step of the reaction, and its isomers enter the next step of the reaction Impurities will be produced. Therefore, we need to take some measures and methods to crystallize and purify compound Ⅰ, thereby increasing its content and laying the foundation for the next reaction. [0006] [0007] Wherein, the R group is Cl or Br. [0008] So far, no li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/20
CPCC07B2200/13C07D307/20
Inventor 陈本顺
Owner 江苏阿尔法集团福瑞药业(宿迁)有限公司