A kind of preparation method of trexagliptin and salt thereof
一种曲格列汀琥珀酸盐、体积比的技术，应用在曲格列汀及其盐的制备领域，能够解决粗品分离纯化步骤繁琐、不适合工业化生产、曲格列汀收率低等问题，达到减少副反应以及杂质化合物的生成、成本低、分离纯化方法简便的效果
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Embodiment 1
[0063] 6-Chloro-3-methyluracil (1.5g), potassium carbonate (3.88g), 2-cyano-5-fluorobenzyl bromide (2.6g) were dissolved in 20mL of DMSO, and the above mixture was heated to 50-60°C for 5h , cooled to 10°C, added 20 mL of water to the reaction solution, a light yellow solid precipitated, filtered, washed the solid with isopropanol, and dried in vacuo to obtain 1.6 g of the product (compound 3);
[0064] Under nitrogen protection, compound 3 (1g, 3.41mmol) was dissolved in 10mL DMSO, stirred until clear, and (Pd(OAc) 2 (7.7mg, 0.034mmol), BINAP (32mg, 0.051mmol), K 3 PO 4 (2.17g, 10.23mmol), the above mixture was heated to 80°C, 3-Boc-aminopiperidine (compound 7, 0.82g, 4.1mmol) was dissolved in 1mL DMSO and added to the above reaction mixture, stirred at 80°C for 5h, TLC Detect the disappearance of compound 3; cool down to room temperature, filter the reaction solution, pour the filtrate into water, extract with dichloromethane, dry the organic phase, and evaporate to drynes...
Embodiment 2
[0074] 6-Chloro-3-methyluracil (30g), potassium carbonate (77.6g), 2-cyano-5-fluorobenzyl bromide (52g) were dissolved in 200mL of DMSO, and the above mixture was heated to 50-60°C for 5h, then cooled After reaching 10°C, 200 mL of water was added to the reaction solution, and a pale yellow solid precipitated out. After filtration, the solid was washed with isopropanol and dried in vacuo to obtain 33 g of the product (compound 3);
[0075] Under nitrogen protection, compound 3 (10g, 34.1mmol) was dissolved in 50mL DMSO, stirred until clear, and Pd(OAc) (77mg, 0.34mmol), BINAP (320mg, 0.51mmol), K 3 PO 4 (21.7g, 102.3mmo), the above mixture was heated to 80°C, 3-Boc-aminopiperidine (compound 7, 8.2g, 40.9mmol) was dissolved in DMSO (10ml) and added to the above reaction mixture, stirred at 80°C for 5h , TLC detects that compound 3 disappears; cool down to room temperature, filter the reaction solution, pour the filtrate into water, extract with dichloromethane, dry the organi...
Embodiment 3
[0079] 6-Chloro-3-methyluracil (3g, 18.8mmol), potassium carbonate (12.9g, 94mmol), 2-cyano-5-fluorobenzyl bromide (6g, 28.1mmol) were dissolved in 60mL of DMSO, and the above mixture was heated React at 50-60°C for 5h, cool down to 10°C, add 60mL of water to the reaction solution, and a pale yellow solid precipitates out. After filtration, the solid was washed with isopropanol and dried in vacuo to obtain 2.8 g of the product (compound 3);
[0080] Under nitrogen protection, compound 3 (2g, 6.8mmol) was dissolved in 20mL DMSO, stirred until clear, and Pd(OAc) (153mg, 0.68mmol), BINAP (622mg, 1mmol), K 3 PO 4 (4.3g, 20.4mmol), the above mixture was warmed to 80°C, (R)-3-Boc-aminopiperidine (compound 7, 2g, 10.2mmol) was dissolved in DMSO (50ml) and added to the above reaction mixture, 80 Stir at ℃ for 5 h, TLC detects that compound 3 disappears; cool down to room temperature, filter the reaction solution, pour the filtrate into water, extract with dichloromethane, dry the or...
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