A kind of preparation method of green caserin hydrochloride hemihydrate crystal form

A green caserin hydrochloride, hemihydrate technology, applied in the direction of organic chemistry, can solve the problems of reducing the optical purity of the product and affecting the quality of the finished product, and achieve the effect of recyclable solvent, simple preparation method and high optical purity.

Active Publication Date: 2017-03-29
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high temperature of this preparation method, the configuration transformation of the target product part occurs, thus resulting in a decrease in the optical purity of the product, thereby affecting the quality of the finished product

Method used

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  • A kind of preparation method of green caserin hydrochloride hemihydrate crystal form
  • A kind of preparation method of green caserin hydrochloride hemihydrate crystal form
  • A kind of preparation method of green caserin hydrochloride hemihydrate crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (a) Preparation of green caserin hydrochloride

[0023] Add 100 mL of dichloromethane (moisture content: 0.1%) to 10.0 g (0.05 mol) of green caserin free base at 0-5 °C, stir until it is clear and completely dissolved, then slowly inject dry hydrogen chloride into the reaction solution After the gas was saturated, dichloromethane was distilled off under reduced pressure at 25°C to obtain 11.5 g of off-white powdery greencaserin hydrochloride solid, with a yield of 97.0%.

[0024] (b) Preparation of green caserin hydrochloride hemihydrate crystal form

[0025] (1) Add 115 mL of dichloromethane (moisture 0.1%) to 11.5 g (0.05 mol) of green caserin hydrochloride at 25-30 °C, stir until clear and completely dissolved, then add 0.45 g (0.025 mol) ) distilled water, stirred for 1.5 hours, concentrated and removed the solvent by distillation under reduced pressure at 25°C to obtain viscous oil.

[0026](2) Cool the viscous oil to 0-5°C, add 173 mL of ethyl acetate dropwise t...

Embodiment 2

[0032] (a) Preparation of green caserin hydrochloride

[0033] Add 1500mL of isopropanol (0.2% water) to 100.0g (0.51mol) greencaserin free base at 0-5°C, stir until clear and completely dissolved, then slowly inject dry hydrogen chloride gas into the reaction solution After saturation, the isopropanol was distilled off under reduced pressure at 30°C to obtain 113.0 g of off-white powdery green caserin hydrochloride solid, with a yield of 95.0%.

[0034] (b) Preparation of green caserin hydrochloride hemihydrate crystal form

[0035] (1) Add 1700mL of isopropanol (0.2% water) to 113.0g (0.487mol) greencaserin hydrochloride at 25-30°C, stir until clear and completely dissolved, then add 5.0g (0.278mol) distilled water, stirred for 1.5 hours, concentrated and removed the solvent by distillation under reduced pressure at 30°C to obtain a viscous oil.

[0036] (2) Cool the viscous oil to 0-5°C, add 2260 mL of n-hexane dropwise to the oil while stirring, and continue stirring at ...

Embodiment 3

[0038] (a) Preparation of green caserin hydrochloride

[0039] Add 500mL of anhydrous methanol (moisture content: 0.1%) to 100.0g (0.51mol) green caserin free base at 0-5°C, stir until clear and completely dissolved, then slowly inject dry hydrogen chloride gas into the reaction solution After saturation, anhydrous methanol was evaporated under reduced pressure at 30°C to obtain 116.3 g of off-white powdery green caserin hydrochloride solid, with a yield of 98.0%.

[0040] (b) Preparation of green caserin hydrochloride hemihydrate crystal form

[0041] (1) Add 600mL of absolute ethanol (0.3% water) to 116.3g (0.5mol) of green caserin hydrochloride at 25-30°C, stir until clear and completely dissolved, then add 5.0g (0.278mol) distilled water, stirred for 1 hour, concentrated and removed the solvent by distillation under reduced pressure at 30°C to obtain a viscous oil.

[0042] (2) Cool the viscous oil to 0-5°C, add 1163 mL of acetone dropwise to the oil while stirring, and ...

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Abstract

The present invention belongs to the preparation method of green caserin hydrochloride hemihydrate crystal form in the field of compound crystal form preparation. The method comprises the following steps: (1) completely dissolving green caserin hydrochloride in the first organic After being put into the solvent, add water, stir, concentrate to remove the solvent to obtain an oily substance; (2) add a second organic solvent to the oily substance, stir to obtain the crystal form of green caserin hydrochloride hemihydrate. The method does not need to control the feeding amount of hydrogen chloride gas and realize the crystal transformation process without heating, and has the advantages of easy control of reaction conditions, mildness, high yield and good quality of the obtained product.

Description

technical field [0001] The invention belongs to the preparation method of green caserin hydrochloride hemihydrate crystal form in the field of compound crystal form preparation. Background technique [0002] With the development of the economy and the improvement of people's living standards, the incidence of obesity is rising rapidly, and it has attracted more and more attention. In the United States, more than 50% of adults and about 25% of children are overweight or obese, and the cost of treating obesity exceeded $70 billion in 1995 alone. The 2002 "Nutrition and Health Survey of Chinese Residents" showed that the overweight and obesity rates of adults in my country were 22.8% and 7.1% respectively. It is estimated that there are about 60 million obese people in China and more than 200 million overweight people. Compared with the 1992 survey, the adult overweight rate increased by 39%, and the obesity rate increased by 97%. Among them, the overweight and obesity rates ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/16
CPCC07D223/16
Inventor 刘丹白跃飞闫妍韩晓丹吴晓璟张晓妍祝春艳胡铁军
Owner NORTHEAST PHARMA GRP
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