Columbamine II derivatives and preparation method and application thereof
A kind of technology of tritylamine and its derivatives in Africa, applied in the field of tritylamine derivatives in Africa and its preparation and application
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Embodiment 1
[0024] Embodiment 1: the synthesis of compound 1 (2-butyl Africa tritylamine hydrobromide)
[0025]
[0026] Weigh 1.13 g of African tetranthylamine (raw material), put it in a 1000 mL round bottom flask, add 25 mL of 1-bromo-n-butane, 53 mL of DMF, 1.2 g of Na 2 CO 3 , magnetically stirred, heated, and refluxed for 24 hours. After TLC detection, a new product was generated [(GF254 plate, developing agent: chloroform: acetone: methanol: ammonia (20:2:1:0.1)], stop the reaction. After AB -8 macroporous adsorption resin chromatography, silica gel column chromatography [eluent: ethyl acetate: dichloromethane: methanol: ammonia water (3:9:2.5:0.5)] separation, methanol recrystallization, that is, identified by hydrogen spectrum As the target compound, it is a new compound, 9.87 (1H, s), 8.99 (1H, s), 8.20 (1H, d, J=9.0Hz), 8.02 (1H, d, J=9.0Hz), 7.7 (1H, s), 7.08(1H, s), 4.93(2H, t, J=6.0Hz), 4.13(2H, t, J=7.5Hz), 4.09(3H, s), 4.06(3H, s), 3.87( 3H, s), 3.21(2H, t, J=6.0Hz),...
Embodiment 2
[0027]Embodiment 2: the synthesis of compound 2 (2-allyl alkyl African tritylamine hydrobromide)
[0028]
[0029] Weigh 1.04 g of African tetranthylamine (raw material), put it in a 1000 mL round bottom flask, add 25 mL of 3-bromoallyl propane, 30 mL of DMF, 1.03 g of Na 2 CO 3 , magnetically stirred, heated, and refluxed for 45 h. After TLC detection, a new product was formed [(GF254 plate, developing solvent: ethyl acetate: dichloromethane: methanol: ammonia water (3:9:2.5:0.5)], stop Reaction. After AB-8 macroporous adsorption resin chromatography, silica gel column chromatography (eluent and developer) separation, methanol recrystallization, that is, the target compound identified by hydrogen spectrum, is a new compound, 9.88 (1H, s) , 9.00(1H, s), 8.20(1H, d, J=9.0Hz), 8.01(1H, d, J=9.0Hz), 7.74(1H, s), 7.11(1H, s), 6.10(1H, m), 5.47 (1H, dd, J=1.5, 16.5Hz), 5.30 (1H, dd, J=1.5, 16.5Hz), 4.91 (2H, t, J=6.0Hz), 4.73 (2H, d, J = 5.0 Hz), 4.09 (3H, s), 3.88 (3H, s), 3...
Embodiment 3
[0030] Embodiment 3: the synthesis of compound 3 (2-ethyl African tritylamine hydrobromide)
[0031]
[0032] Weigh 1.01 g of tritylamine (raw material), put it in a 100 mL round bottom flask, add 10 mL of 1-bromoethane, 50 mL of DMF, 1.32 g of Na 2 CO 3 , magnetic stirring, heating, and reflux reaction for 50 h. After TLC detection, a new product was formed [(GF254 plate, developing solvent: chloroform: acetone: methanol: ammonia water (3:9:2.5:0.5)], stop the reaction. After AB -8 Macroporous adsorption resin chromatography, silica gel column chromatography (eluent and developer) separation, methanol recrystallization, that is, the target compound was identified by hydrogen spectrum, it is a new compound, 9.87 (1H, s, H-8) , 9.01(1H, s, H-13), 8.20(1H, d, J=9.5Hz, H-12), 8.02(1H, d, J=9.5Hz, H-11), 7.70(1H, s, H-1), 7.09(1H, s, H-4), 4.94(2H, t, J=6.0Hz), 4.19(2H, q, J=7.0Hz), 4.09(3H, s), 4.06(3H , s), 3.87 (3H, s), 3.22 (2H, q, J=6.0Hz), 1.40 (2H, t, J=6.0Hz); yield ...
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