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
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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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