Pseudoephedrine derivative and preparation method and application thereof
A kind of technology of ephedrine and derivatives, applied in the field of pseudoephedrine derivatives and preparation thereof
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Embodiment 1
[0039] 1,6-bis((S)-2-(methylamino)propyl)isochroman-3-one (Ia-1,R 1 =R 2 =CH 3 )
[0040] Weigh 1.71g of 2-(5-chloro-2-methylphenyl)ethan-1-ol into a 150mL three-necked flask, measure 20mL of acetonitrile, stir and dissolve at room temperature, add 0.4g of glucose isomerase , 0.2g of chromium trioxide, continue to stir at room temperature for 10min, weigh 2.28g of periodic acid and dissolve in 10mL of acetonitrile, gradually and slowly dropwise add to the reaction system, and continue to react at room temperature for 36h. After the reaction of Ia-1 was completed, the reaction was stopped, and the solvent was concentrated under reduced pressure. Through column chromatography, the developer was acetone:ether=1:5, and Ia-2 was obtained, 1.32g (yield 66.3%).
[0041] Weigh 1.99g of 2-(5-chloro-2-formylphenyl)acetic acid (Ia-2) into a 150mL round bottom flask, measure 20mL of ethanol, stir and dissolve at room temperature, add 1.83g of N -Dimethylpropan-2-amine, add 0.5g of α-a...
Embodiment 2
[0045] 1,6-bis((S)-2-(methylamino)butyl)isochroman-3-one (R 1 =CH 3 , R 2 =CH 2 CH 3 )
[0046] The preparation method is as in Example 1, except that N-methylbutan-2-amine is used. White solid, mp: 216~220℃, MSm / z: 341.46 (M+Na); 1 H-NMR (DMSO-d 6 , ppm) δ: 7.42~7.09 (m, 3H), 6.85 (m, 1H), 3.52~3.49 (d, 2H), 3.12~3.06 (m, 4H), 2.93~2.54 (m, 4H), 1.92~ 1.48 (m, 2H), 0.87 (t, 2H); 13 C-NMR (DMSO-d 6 , ppm) δ: 167.4, 138.1, 137.3, 135.4, 132.5, 130.9, 125.3, 68.9, 67.9, 66.4, 58.4, 42.2, 39.9, 36.9, 34.0, 27.8, 10.7.
Embodiment 3
[0048] 1,6-bis((S)-2-(ethylamino)butyl)isochroman-3-one (R 1 =R 2 =CH 2 CH 3 )
[0049] The preparation method is the same as in Example 1, except that N-diethylbutyl-2-amine is used. White solid, mp: 201~215°C, MSm / z: 347.09 (M+H), 369.26 (M+Na); 1 H-NMR (DMSO-d 6 , ppm) δ: 7.37~7.18(m, 3H), 5.72(m, 1H), 3.52~3.38(m, 4H), 2.91(d, 1H), 2.79(d, 1H), 2.59~2.54(m, 3H), 2.13(m, 1H), 1.97~1.53(m, 4H), 1.11(s, 2H), 0.84(t, 2H); 13 C-NMR (DMSO-d 6 , ppm) δ: 169.4, 138.1, 136.7, 135.4, 130.5, 128.7, 126.9, 66.6, 62.4, 55.9, 42.2, 40.1, 36.9, 28.6, 27.4, 15.9, 10.3.
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