Crystalline form of eliglustat hemitartrate, process for preparation and pharmaceutical composition containing said crystalline form
A kind of hemi-tartrate, the form of technology, used in the field of medicine
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Embodiment 1
[0039] Example 1: Referring to the example of patent CN201510703628.2, to synthesize eliglustat, the specific steps are as follows.
[0040] 1. Preparation of the compound of formula (Ⅲ)
[0041] Add the compound of formula (II) (278g, 1mol) and acetonitrile (2.8L) into a 5L round-bottom three-necked flask equipped with a drying tube, add potassium carbonate (276g, 2mol) under stirring, and add Boc anhydride dropwise in an external bath at 10°C (327g, 1.5mol) in acetonitrile (300mL) solution, continue to react for 3h after addition, then add water (3L), extract three times with ethyl acetate (800mL×3), combine organic phases, wash with saturated brine (800mL) Wash, dry over anhydrous sodium sulfate, filter, and concentrate to obtain 368 g of light yellow oil, with a yield of 97.6%.
[0042]
[0043] 2. Preparation of the compound of formula (Ⅳ)
[0044] In a 5L round-bottom three-neck flask equipped with a drying tube, add the compound of formula (Ⅲ) (302g, 0.8mol) and DM...
Embodiment 2
[0055] Example 2: Preparation of Eliglustat Hemitartrate Crystals
[0056] At room temperature, the eligrusastat (10 g / 24.7 mmol) prepared in Example 1 was dissolved in 140 ml of methanol / acetone (v / v: 0.05:0.95) solution. Take L-tartaric acid (1.84g / 12.3mmol) and add it to 60ml of methanol / acetone (v / v: 0.05:0.95) solution, heat to 40°C, the solid is completely dissolved, and drop this solution into the former solution. After stirring at room temperature for ten minutes, a small amount of solids slowly precipitated out, and after fifteen minutes, a large amount of solids precipitated out. After stirring for another 3 hours, it was filtered, and the filter cake was rinsed with 20ml*2 acetone, and the solids were vacuum-dried at 50°C for 16-20 hours to obtain Off-white solid 9.18g, yield 77.5%.
Embodiment 3
[0057] Example 3: Preparation of Eliglustat Hemitartrate Crystals
[0058] At room temperature, the eligrusastat (10 g / 24.7 mmol) prepared in Example 1 was dissolved in 140 ml of water / acetone (v / v: 0.01:0.99) solution. Take L-tartaric acid (1.84g / 12.3mmol) and add it to 60ml of water / acetone (v / v: 0.01:0.99) solution, heat to 40°C, the solid is completely dissolved, and drop this solution into the former solution. After stirring at room temperature for ten minutes, a large amount of solid precipitated rapidly. After stirring for another 3 hours, it was filtered, rinsed with 2*20ml of acetone, and the solid was vacuum-dried at 60°C for 16-20 hours to obtain 9.78g of off-white solid, with a yield of 82.5%.
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