Oseltamivir preparation method
An oseltamivir and reaction technology, applied in the field of drug synthesis, can solve problems such as uneconomical and long reaction time, and achieve the effects of cost saving, reaction time reduction and high yield
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Embodiment 1
[0032] Add ethyl (3R,4R,5S)-4-acetamido-5-azido-3-(1-ethylpropoxy)-1-cyclohexene-1-carboxylate into a 100mL reaction flask 100mg, 5mg Lindlar catalyst, add hydrogen, the pressure is 0.5atm, react at room temperature for 3h. After the reaction, the reaction solution was filtered, and the solvent in the filtrate was evaporated to dryness to obtain 90.74 mg of the product with a yield of 98%.
[0033] MS(m / z):[M+H] + 313.1,[2M+H] + 625.3
[0034] 1 HNMR (400MHz, CD 3 OD)δ6.77(s,1H),4.21(q,J=7.1Hz,2H),4.09–4.04(m,1H),3.69(dd,J=10.8,8.8Hz,1H),3.42-3.34( m,1H),2.88(td,J=10.4,5.4Hz,1H),2.78(dd,J=17.7,5.2Hz,1H),2.20–2.09(m,1H),2.02(s,3H),1.57 -1.46 (m, 4H), 1.29 (t, J=7.1Hz, 3H), 0.92 (t, J=6.1Hz, 3H), 0.89 (t, J=6.2Hz, 3H). The proton nuclear magnetic resonance spectrum was determined by Bruker ARX-400 nuclear magnetic resonance instrument, and the liquid phase mass spectrometry was determined by Waters QuattromicroAPI triple quadrupole mass spectrometer (equipped with electro...
Embodiment 2
[0036] Add ethyl (3R,4R,5S)-4-acetamido-5-azido-3-(1-ethylpropoxy)-1-cyclohexene-1-carboxylate into a 100mL reaction flask 100mg, 5mg Lindlar catalyst, add hydrogen, the pressure is 0.5atm, react at room temperature for 3h. After the reaction was finished, the reaction solution was filtered, and the solvent in the filtrate was evaporated to dryness to obtain 90.27 mg of product with a yield of 97.8%. The verification method is the same as in Example 1.
Embodiment 3
[0038] Add ethyl (3R,4R,5S)-4-acetamido-5-azido-3-(1-ethylpropoxy)-1-cyclohexene-1-carboxylate into a 100mL reaction flask 150mg, 7.5mg Lindlar catalyst, add hydrogen, the pressure is 0.5atm, react at room temperature for 3h. After the reaction, the reaction solution was filtered, and the solvent in the filtrate was evaporated to dryness to obtain 136.4 mg of the product with a yield of 98.5%. The verification method is the same as in Example 1.
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