Acid absorbing agent for preparing cinchona alkaloids ligand
A technology for cinchona alkaloids and ligands, which is applied in the field of acid binding agents, can solve the problems of difficulty in accurate quantification, danger, easy combustion, etc., and achieves the effects of avoiding the column chromatography process, easy operation and safe use.
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Embodiment 1
[0030] Example 1: Synthesis of Ligand 1
[0031] Add 0.295g (0.0015mol) 1,4-dichloro-2,3-naphthyridine, 0.975g (0.003mol) dihydroquinine, 0.63g (0.015mol) CaH 2 , 4.5mL DMF, N 2 Protected, reacted at 90°C, the reaction solution was a light yellow turbid solution, the reaction process was monitored by TLC until the raw materials disappeared, and the reaction time was 1 h in total. Add 10mL ethyl acetate and 5mL water and stir, separate the water layer, extract with ethyl acetate (15mL×3), combine the organic phases, anhydrous MgSO 4 dry. After filtering and concentrating under reduced pressure to leave about 3 mL of liquid, white needle-like crystals precipitated out, dried, and washed with a little anhydrous ether to obtain white crystals, with a yield of 95%. m.p.133~135℃. 1 HNMR (CDCl 3 , internal standard TMS): δ8.65(d, J=4.6Hz, 2H), 8.33(m, 2H), 7.98(d, J=9.2Hz, 2H), 7.96(m, 2H), 7.56(d, 2H), 7.44(d, J=4.7Hz, 2H), 7.36(d, 1H), 7.35(d, 1H), 7.01(d, 2H), 3.9(s, 6H), 3....
Embodiment 2
[0032] Embodiment 2: the synthesis of ligand 2
[0033] In a 100mL three-necked flask, add 0.295g (0.0015mol) 1,4-dichloro-2,3-naphthyridine, 0.975g (0.003mol) dihydroquinidine, 0.63g (0.015mol) CaH 2 , 4.5mL N, N-dimethylformamide (DMF), N 2 Protected, reacted at 90°C, the reaction solution was a light yellow turbid solution, the reaction process was monitored by TLC until the raw materials disappeared, and the reaction time was 5 hours in total. Add 10mL ethyl acetate and 5mL water and stir, separate the water layer, extract with ethyl acetate (15mL×3), combine the organic phases, anhydrous MgSO 4 dry. After filtering and concentrating under reduced pressure to leave about 3 mL of liquid, white needle-like crystals precipitated out, dried, and washed with a little anhydrous ether to obtain white crystals with a yield of 78%. m.p.176-178°C. 1 H NMR (CDCl 3 , internal standard TMS): δ8.65(d, J=5.3Hz, 2H), 8.33(m, 2H), 7.98(d, J=9.2Hz, 2H), 7.94(m, 2H), 7.58(d, 2H), 7.43(...
Embodiment 3
[0034] Embodiment 3: the synthesis of ligand 3
[0035] Add 0.295g (0.0015mol) 1,4-dichloro-2,3-naphthalene, 0.97g (0.003mol) quinine, 0.63g (0.015mol) CaH to a 100mL three-necked flask 2 , 4.5mL DMF, N 2Protected, reacted at 90°C, the reaction solution was a light yellow turbid solution, the reaction process was monitored by TLC until the raw materials disappeared, and the reaction time was 6 hours in total. Add 10mL ethyl acetate and 5mL water and stir, separate the water layer, extract with ethyl acetate (15mL×3), combine the organic phases, anhydrous MgSO 4 dry. After filtering and concentrating under reduced pressure to leave about 3 mL of liquid, white needle-like crystals precipitated out, dried, and washed with a little anhydrous ether to obtain white crystals, with a yield of 95%. m.p.160~161℃. 1 H NMR (CDCl 3 , internal standard TMS): δ8.65 (d, J=5.3Hz, 2H, Ar-H), 8.33 (m, 2H, Ar-H), 7.98 (d, J=9.2Hz, 2H, Ar-H) , 7.96(m, 2H, Ar-H), 7.58(s, 2H, Ar-H), 7.44(d, J=...
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