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A kind of crystal form of hepatitis B surface antigen inhibitor and its application

A technology of crystal form and acetonitrile, which is applied in the application field of preparing hepatitis B surface antigen inhibitors, can solve the problems such as poor curative effect of HBsAg

Active Publication Date: 2022-05-03
푸지엔에이키링크바이오테크놀로지컴퍼니리미티드
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing clinical therapies are not effective in reducing HBsAg. Therefore, the development of small-molecule oral inhibitors that can effectively reduce HBsAg is urgently needed in clinical medicine.

Method used

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  • A kind of crystal form of hepatitis B surface antigen inhibitor and its application
  • A kind of crystal form of hepatitis B surface antigen inhibitor and its application
  • A kind of crystal form of hepatitis B surface antigen inhibitor and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Embodiment 1: the preparation of formula (I) compound

[0065]

[0066] Step A: Dissolve 1-1 (10.00 g, 59.5 mmol) in dichloromethane (500 ml) at 0°C, then add sulfuryl chloride (10.77 g, 79.77 mmol, 7.98 ml), and the mixed solution was dissolved at 35 Stir at °C for 38 hours. The solution was then poured into 300 ml of saturated aqueous sodium bicarbonate solution and stirred and separated. The aqueous phase was extracted with ethyl acetate (150 mL*3 times), then the combined organic phases were washed with saturated brine (40 mL*3 times), dried over anhydrous sodium sulfate, and distilled under reduced pressure to obtain a white residue thing. Then the white residue was purified by silica gel column chromatography (eluent: petroleum ether / ethyl acetate=30 / 1 to 20 / 1) to obtain compound 1-2.

[0067] 1 H NMR (400MHz, MeOH-d 4 )δ10.75(s,1H),7.74(s,1H),6.54(s,1H),5.98(s,1H),3.85(s,3H).

[0068] Step B: 1-2 (8.00 g, 39.49 mmol), 1-bromo-3-methoxy-propane (7.25 g, 4...

Embodiment 2

[0080] Embodiment 2: Preparation of formula (I) compound A crystal form

[0081] Control the temperature at 40°C, add the compound of formula (I) (1g) into the reaction flask, then add acetone (10mL), stir the mixture at 40°C for 24 hours, cool to room temperature and filter, the filter cake is washed with acetone (10mL) , the crude product was obtained, and the crude product was dried in a vacuum oven (45°C, 16 hours) to obtain the compound A crystal form of formula (I).

Embodiment 3

[0082] Embodiment 3: solid stability test of formula (I) compound A crystal form under high temperature and high humidity conditions

[0083] Weigh 2 samples of compound A crystal form of formula (I) in parallel, about 100 mg each, place them at the bottom of the glass sample bottle, and spread them into a thin layer. The sample was sealed with aluminum foil, and some small holes were pierced on the aluminum foil to ensure that the sample could fully contact with the ambient air, and placed in a constant temperature and humidity chamber at 40°C / 75% humidity. The samples placed under the above conditions were sampled and detected on the 5th and 10th days, and the test results were compared with the initial test results on day 0. The test results are shown in Table 2 below:

[0084] Table 2 Solid stability test of crystal form A under high temperature and high humidity conditions

[0085] Time point (day) Exterior crystal form purity(%) Total impurities (%) ...

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Abstract

The invention discloses a crystal form of the hepatitis B surface antigen inhibitor and a preparation method thereof, and also includes the application of the crystal form in the preparation of the hepatitis B surface antigen inhibitor.

Description

technical field [0001] The invention relates to a crystal form of the hepatitis B surface antigen inhibitor and a preparation method thereof, and also includes the application of the crystal form in the preparation of the hepatitis B surface antigen inhibitor. Background technique [0002] Hepatitis B virus, referred to as hepatitis B, is a disease caused by hepatitis B virus (Hepatitis B Virus, HBV) infection after the body. Hepatitis B virus is a hepatotropic virus that mainly exists in liver cells and damages liver cells, causing inflammation, necrosis, and fibrosis of liver cells. There are two types of hepatitis B: acute and chronic. Most acute hepatitis B can be cured by its own immune mechanism in adults. However, chronic hepatitis B (CHB) has become a great challenge to global health care, and it is also the main cause of chronic liver disease, cirrhosis and hepatocellular carcinoma (HCC). It is estimated that 2 billion people in the world are infected with chroni...

Claims

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Application Information

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IPC IPC(8): C07D498/04A61P31/20
CPCC07D498/04A61P31/20C07B2200/13A61K31/5365
Inventor 蔡哲孙飞丁照中
Owner 푸지엔에이키링크바이오테크놀로지컴퍼니리미티드
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