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Crystal forms of tricyclic compounds and their applications

A compound and crystal form technology, applied in the field of preparation of drugs for the treatment of HBV-related diseases, can solve the problems of high cost and easy recurrence

Active Publication Date: 2022-05-27
푸지엔에이키링크바이오테크놀로지컴퍼니리미티드
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no specific drug for the treatment of hepatitis B in the world. The first-line drugs for the treatment of hepatitis B in China are mainly nucleoside drugs, interferon and traditional Chinese medicine, but there are problems such as high cost and easy recurrence. Therefore, new types of anti-hepatitis B drugs have been developed. drug imperative

Method used

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  • Crystal forms of tricyclic compounds and their applications
  • Crystal forms of tricyclic compounds and their applications
  • Crystal forms of tricyclic compounds and their applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Example 1 Preparation of compound of formula (I)

[0076]

[0077] synthetic route:

[0078]

[0079]

[0080] Step 1: Synthesis of Compound 1-A

[0081] Anhydrous dichloromethane (5L) was added to a dry 10L there-necked flask, stirring was started, compound 1-SMA (500.00 g) and nitromethane were added to the there-necked flask in turn, the system was placed in a dry ice ethanol bath, and cooled to -10°C. Control the temperature -10°C-0°C, slowly add aluminum trichloride (1.15kg) into the reaction flask, control the temperature to be less than -0°C, slowly add α,α-dichlorodimethyl methyl ether (495.00g) It was added to the reaction kettle and slowly raised to room temperature, and stirred for 18 hours. As monitored by TLC (PE:EA 3:1), the starting point disappeared and a new point with greater polarity was formed. The reaction solution was drawn out, slowly added dropwise to 10% potassium hydrogen sulfate solution (3 L), stirred for 20 minutes, and crushed i...

Embodiment 2

[0122] Example 2 Preparation of Form A of the Compound of Formula (I)

[0123] 35 mg of the compound of formula (I) was weighed into a 1.5 mL liquid phase vial, 400 μL of tert-butyl methyl ether was added, and sonicated to mix or dissolve. The suspension sample was placed on a constant temperature shaker (40°C) and stirred (protected from light) for 3 days. Then, the sample liquid was centrifuged rapidly, and the centrifuged solid was dried in a vacuum drying oven at 30° C. for 5 hours, and the obtained dried sample was subjected to XRPD detection to obtain the A crystal form of the compound of formula (I).

Embodiment 3

[0124] Example 3 Preparation of B crystal form of compound of formula (I)

[0125] 35 mg of the compound of formula (I) was weighed into a 1.5 mL liquid phase vial, 400 μL of acetone was added, and sonicated or dissolved. The suspension sample was placed on a constant temperature shaker (40°C) and stirred (protected from light) for 3 days. Then, the sample liquid was centrifuged rapidly, and the centrifuged solid was dried in a vacuum drying oven at 30° C. for 5 hours. The obtained dried sample was subjected to XRPD detection to obtain the B crystal form of the compound of formula (I).

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Abstract

The invention discloses crystal form A and crystal form B of the compound represented by formula (I), and the application thereof in the preparation of medicines for treating HBV-related diseases.

Description

[0001] This application claims the priority of Chinese patent application CN2018109690068 with an application date of August 23, 2018. This application cites the full text of the Chinese patent application. technical field [0002] The present invention relates to the A crystal form and the B crystal form of the compound represented by formula (I), and their application in the preparation of medicines for treating HBV-related diseases. Background technique [0003] Hepatitis B is an inflammatory reaction caused by the invasion of hepatitis B virus, which can lead to a series of problems such as liver pain, hepatosplenomegaly, liver fibrosis, and even liver cirrhosis and even liver cancer in severe cases. According to statistics, there are about 350-400 million hepatitis B virus carriers in the world, of which 1 / 3 of the carriers are in China, and the number of deaths caused by hepatitis B in China is as high as 500,000 every year. [0004] At present, there is no specific d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/00A61K31/33A61K31/395A61K31/40A61P1/16
CPCA61P1/16C07D513/04A61K31/554A61P31/20C07B2200/13
Inventor 王静江志赶贺海鹰杨亚讯
Owner 푸지엔에이키링크바이오테크놀로지컴퍼니리미티드