Amide-chaoger base derivatives and their synthesis methods and applications
A technology of Chaoger base and synthesis method, applied in the field of amide-Chaoger base derivatives and synthesis thereof, can solve the problems of complicated synthesis steps, high catalyst toxicity, large catalyst amount, etc., and achieves mild reaction conditions and reaction time. Short, high-yield effects
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0037] The synthesis of embodiment 1 amide-chaoger base derivative 3a, 3b
[0038]
[0039] Azacyclic amine 2 (2mmol) and sodium hydride (60% paraffin mixture, 4mmol) were added to a dry two-necked flask, anhydrous tetrahydrofuran (10mL) was added under argon protection, and the reaction was stirred at room temperature for 2h, and intermediate 1 ( 1mmol) was dissolved in 5mL of anhydrous tetrahydrofuran, and then the solution was slowly dripped into a double-necked flask, transferred to an oil bath after the dripping, and heated to reflux for 24h under the protection of argon (TLC tracking). The solvent was evaporated to dryness under reduced pressure, and water was added with 1M NaHSO 4 The pH of the solution was adjusted to neutrality, extracted three times with dichloromethane (100 mL each time), the combined organic phases were dried over anhydrous sodium sulfate, and the solvent was spin-dried to obtain a crude product, which was purified by column chromatography (V 乙...
Embodiment 2
[0040] The synthesis of embodiment 2 amide-chaoger base derivatives 3c, 3d, 3e, 3f
[0041]
[0042] Add azacyclic amine 2 to the dry two-necked flask a (2mmol), sodium hydride (60% paraffin mixture, 4mmol), add anhydrous tetrahydrofuran (10mL) under argon protection, stir and react at room temperature for 2h, dissolve intermediate 1 (1mmol) in 5mL anhydrous tetrahydrofuran, and then The solution was slowly dripped into a double-necked bottle, and then transferred to an oil bath, and heated to reflux for 24 hours under the protection of argon (TLC tracking). The solvent was evaporated to dryness under reduced pressure, and water was added with 1M NaHSO 4 The pH of the solution was adjusted to neutrality, extracted three times with dichloromethane (100 mL each time), the organic phases were combined, dried over anhydrous sodium sulfate, and the solvent was spin-dried to obtain a crude product, which was purified by column chromatography (V 乙酸乙酯 :V 甲醇 =5:1), the pure produ...
Embodiment 3
[0043] The synthesis of embodiment 3 amide-chaoger base derivative 3g, 3h
[0044]
[0045] Add azacyclic amine 2 to the dry two-necked flask b (2mmol), sodium hydride (60% paraffin mixture, 4mmol), under the protection of argon, add anhydrous DMF (10mL), stir the reaction at room temperature for 2h, dissolve intermediate 1 (1mmol) in 5mL anhydrous DMF, and then The solution was slowly dropped into a double-necked bottle, and then transferred to an oil bath, and heated at 100°C for 24h under the protection of argon (TLC tracking). The solvent was evaporated to dryness under reduced pressure, and water was added with 1M NaHSO 4 The solution is adjusted to neutral pH, and the crude product is obtained by filtration, and purified by column chromatography (V 乙酸乙酯 :V 甲醇 =5:1), the pure product 3g or 3h was obtained.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More