Romidepsin acetate crystal form and preparation method thereof

[0083] At a constant temperature of 25°C, weigh 4g of romidepsin and dissolve it in 10ml of acetic acid, and ultrasonically assist in dissolving. After 24 hours, crystals were found to be precipitated, and romidepsin acetate crystals were obtained by filtration to obtain romidepsin acetate crystal form with a purity of 99.1% and a yield of 85.5%.

[0085] At a constant temperature of 70°C, weigh 5.5g of romidepsin and dissolve it in 10ml of acetic acid, and ultrasonically assist the dissolution. After the romidepsin is completely dissolved, filter through filter paper to obtain a clear solution, and then place the solution at room temperature at 25°C. After 48 hours, crystals were found to be precipitated, and romidepsin acetate crystals were obtained by filtration to obtain romidepsin acetate crystal form with a purity of 99.3% and a yield of 80.5%. Use it for XRPD, DSC, and single crystal detection, see the XRPD spectrum figure 1 , IR spectrum see figure 2 , see the DSC spectrum image 3 , the ellipsoid diagram of the three-dimensional structure of the molecule is shown in Figure 4 , the unit cell packing projection along the a-axis is shown in Figure 5 , the XRPD of the initial romidepsin acetate crystal form and the XRPD of the sample after 60 days see Figure 6 , the comparison of its XRPD pattern with the romid

[0087] At a constant temperature of 45°C, weigh 4.5g of romidepsin and dissolve it in 10ml of acetic acid, and ultrasonically assist the dissolution. After the romidepsin is completely dissolved, filter through filter paper to obtain a clear solution, and then place the solution at room temperature at 10°C. After 48 hours, crystals were found to be precipitated, and romidepsin acetate crystals were obtained by filtration to obtain romidepsin acetate crystal form with a purity of 99.2% and a yield of 87.3%.