Highly substituted alpha-amino phosphonate derivative as well as preparation method and medical application thereof
A technology of monoethyl methylphosphonate and diethyl methylphosphonate, which is applied in the fields of highly substituted α-aminophosphonic acid derivatives, their preparation and their medical application, and can solve the lack of prevention of autoimmune diseases and/or treatments, immunocompromised, Cushing's syndrome, etc.
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Embodiment 1
[0099] Example 1: Preparation of α-[3-(cyclohexylamino)propylamino]-α-(2-hydroxy-5-nitrophenyl)methylphosphonic acid monoethyl ester-compound 1
[0100] Take by weighing 9.60g (0.052mol) 5-nitrosalicylaldehyde i.e. 2-hydroxyl-5-nitrobenzaldehyde, 7.85g (0.050mol) N-(3-aminopropyl) cyclohexylamine i.e. [3-( Cyclohexylamino) propylamine] and 7.80g (0.056mol) of diethyl phosphite were dissolved in 50ml of absolute ethanol, stirred at a bath temperature of about 60°C for 2.5 days, cooled, yellow crystals were precipitated, dried to obtain 19.20g, and Yield 92.4%, mp 192-194°C (dec.).
[0101] 1 H-NMR (D 2 O, ppm) 0.922(t, J=7.00Hz, 3H), 0.92-1.22(m, 5H), 1.430(m→d, J=11.76Hz, 1H), 1.588(br-s, 2H), 1.795( m, 4H), 2.60-2.70(m, 1H), 2.70-2.80(m, 1H), 2.82-2.92(m→d, J=9.38Hz, 3H), 3.563(m, 2H), 4.204(d, J=17.85Hz, 1H), 6.548(d, J=8.96Hz, 1H), 7.995(dd, J1=8.96Hz, J2=2.94Hz, 1H), 7.970(d, J=2.94Hz, 1H).
Embodiment 2
[0102] Example 2: Preparation of α-[3-(cyclohexylamino)propylamino]-α-(2,4-dihydroxyphenyl)methylphosphonic acid monoethyl ester-compound 2
[0103] According to the method of Example 1, 2,4-dihydroxybenzaldehyde was used instead of 5-nitrosalicylaldehyde to obtain yellow needle-like crystals with a yield of 91.9%, and mp>300°C.
[0104] 1 H-NMR (D 2O, ppm) 0.916(t, J=7.00Hz, 3H), 0.92-1.14(m, 5H), 1.423(m→d, J=12.32Hz, 1H), 1.52-1.68(m, 4H), 1.791( br-s, 2H), 2.40-2.49(m, 1H), 2.50-2.59(m, 1H), 2.75-2.90(m, 3H), 3.515(m, 2H), 3.821(d, J=18.21Hz, 1H), 6.17(d, J=2.52Hz, 1H), 6.220(dd, J 1 =8.40Hz,J 2 =2.52Hz, 1H), 6.840(dd, J 1 =8.40Hz,J 2 = 1.96Hz, 1H).
Embodiment 3
[0105] Example 3: Preparation of monomethyl α-[2-(dimethylamino)ethylamino]-α-(2-hydroxy-5-nitrophenyl)methylphosphonate-compound 3
[0106] According to the method of Example 1, 2-dimethylaminoethylamine is used to replace N-(3-aminopropyl) cyclohexylamine, and dimethyl phosphite is used to replace diethyl phosphite for reaction to obtain yellow cluster needles Like crystals, yield 93.1%, mp 176-178°C.
[0107] 1 H-NMR (D 2 O, ppm) 2.070(m, 2H), 2.753(s, 6H), 2.84-2.96(m, 2H), 3.325(d, J=10.08Hz, 3H), 3.937(d, J=20.59Hz, 1H) , 6.869(d, J=8.96Hz, 1H), 7.985(dd, J 1 =8.96Hz,J 2 =2.66Hz, 1H), 8.305(d, J=2.66Hz, 1H).
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