2-substituted-6,7-dimethoxy tetralin isoquinoline derivative, preparation method thereof, medicinal composition and application thereof
The technology of a drug and a compound is applied in the application field of preparing a drug for treating diabetes, and can solve problems such as inactivation of GLP-1
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Embodiment 1
[0062] 6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline, English translation: 6,7-dimethoxy-1,2,3,4-tetrahydr roisoquinoline
[0063] 9.05g (0.05mol) of 3,4-dimethoxyphenethylamine and 1.8g of paraformaldehyde were respectively dissolved in 30ml of absolute ethanol, stirred at room temperature for 1-2h, TLC detected the formation of Schiff base, and then added 6N concentrated After adjusting the pH to 3 with hydrochloric acid, the reaction was heated under reflux for 6 hours, a large amount of white solids precipitated, cooled and filtered, and recrystallized from 95% ethanol to obtain 7.92 g of colorless flaky crystals, mp: 254°C. Add the colorless crystals obtained above into 50 ml of 2M sodium hydroxide solution, stir, extract three times with dichloromethane, combine the organic layers, wash the organic layer three times with saturated brine, and dry over anhydrous sodium sulfate. Concentrate to obtain 6.6g of yellow-white solid, yield 68.3%, mp: 81-83°C, literature: 84-85°C ...
Embodiment 2
[0076] 6,7-dimethoxy-2-[N-(N-(4-methylphenyl)acetamide)aminoethyl]-1,2,3,4-tetrahydroisoquinoline (Ia 2 ), English translation: 2-((2-(6,7-dimethoxy-3,4-dihydroisoquinolin-2(1H)-yl)ethyl)amino)-N-(p-tolyl)acetamide
[0077] 0.4g (0.0015mol) 2-(2-aminoethyl)-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride, anhydrous potassium carbonate 0.42g (0.003 mol), 0.18g (0.001mol) N-chloroacetyl-4-methylaniline, according to (Ia 1 ) method to obtain 0.15 g of white solid, yield 39.1%, mp: 92-94°C.
[0078] IR (cm -1 ): 3281, 2972, 1726, 1298, 1189 1 HNMR (CDCl 3 , 500MHz) δ: 9.48 (s, 2H, -NH), 7.43-7.46 (d, 2H, Ar-H), 7.03-7.06 (d, 2H, Ar-H), 6.60 (s, 1H, Ar-H ), 6.47(s, 1H, Ar-H), 3.81-3.85(2s, 6H, 2-OCH 3 ), 3.70 (s, 2H, C1-CH 2 ), 3.44 (s, 2H, -CH 2 ), 2.88-2.93 (m, 6H, -N-CH 2 -CH 2 -NH, C4-CH 2 ), 2.77-2.79(t, 2H, C3-H), 2, 28(s, 3H, -CH 3 )
[0079]MS (ESI, m / z): 384 ([M+1] + , basepeak)
Embodiment 3
[0081] 6,7-dimethoxy-2-[N-(N-4-fluorophenyl)acetamide)aminoethyl]-1,2,3,4-tetrahydroisoquinoline (Ia 3 ), English translation: 2-((2-(6,7-dimethoxy-3,4-dihydroisoquinolin-2(1H)-yl)ethyl)amino)-N-(4-fluorophenyl)acetamide
[0082] 0.4g (0.0015mol) 2-(2-aminoethyl)-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride, anhydrous potassium carbonate 0.42g (0.003 mol), 0.19g (0.001mol) N-chloroacetyl-4-fluoroaniline, according to (Ia 1 ) method to obtain white solid 0.16g, yield 41.3%, mp: 88-90°C.
[0083] IR (cm -1 ): 3290, 2928, 1685, 1405, 1222 1 HNMR (CDCl 3 , 300MHz) δ: 9.63 (s, 1H, -NH), 7.44-7.49 (m, 2H, Ar-H), 6.88-6.94 (m, 2H, Ar-H), 6.59 (s, 1H, Ar-H ), 6.47(s, 1H, Ar-H), 3.82-3.86(2s, 6H, 2-OCH 3 ), 3.58(s, 2H, C1-CH 2 ), 3.40 (s, 2H, -CH 2 ), 2.76-2.89 (m, 6H, -N-CH 2 -CH 2 -NH, C4-CH2), 2.64-2.68 (t, 2H, C3-H) MS (ESI, m / z): 388 ([M+1] + , basepeak)
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