Application of composition of O-(triazolyl) ethyl of Schiglautone A and O-(2-methyl sulfonium ethyl) amido) ethyl derivative in low red blood cell anemia resisting drugs
A low red blood cell and composition technology, applied in the field of preparation and composition, can solve the problems of insufficient hematopoietic raw materials or utilization obstacles
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Embodiment 1
[0030] The preparation of embodiment 1 compound Schiglautone A
[0031] The preparation method of compound Schiglautone A (I) refers to the literature published by Fan-Yu Meng et al. of Schisandra glaucescens. Organic Letters 13 (2011) 1502–1505).
[0032]
Embodiment 2
[0033] The synthesis of the O-bromoethyl derivative (II) of embodiment 2 Schiglautone A
[0034] Compound I (502 mg, 1.00 mmol) was dissolved in 15 mL of benzene, and tetrabutylammonium bromide (TBAB) (0.08 g), 1,2-dibromoethane (7.520 g, 40.00 mmol) and 6 mL of 50% sodium hydroxide solution. The mixture was stirred at 35 °C for 8 h. After 8 hours, the reaction solution was poured into ice water, extracted twice with dichloromethane immediately, and the organic phase solutions were combined. Then the organic phase solution was washed with water and saturated brine three times successively, then dried with anhydrous sodium sulfate, and finally concentrated under reduced pressure to remove the solvent to obtain a crude product. The crude product was purified by silica gel column chromatography (mobile phase: petroleum ether / acetone=100:1.0, v / v), the brown concentrated elution band was collected and the solvent was evaporated to obtain a brown powder of Compound II (508mg, 71%...
Embodiment 3
[0039] The synthesis of the O-(triazolyl) ethyl derivative (III) of embodiment 3 Schiglautone A
[0040] Compound II (358 mg, 0.5 mmol) was dissolved in 10 mL of acetonitrile, anhydrous potassium carbonate (345 mg, 2.5 mmol), potassium iodide (84 mg, 0.5 mmol) and 1,2,3-triazole (2760 mg, 40 mmol) were added thereto ), the mixture was heated to reflux for 3h. After the reaction, the reaction solution was poured into ice water, extracted twice with an equal amount of dichloromethane, and the organic phases were combined. The combined organic phases were successively washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to remove the solvent to obtain a crude product. The crude product was purified by silica gel column chromatography (mobile phase: petroleum ether / acetone=100:1.0, v / v), and the light yellow concentrated elution band was collected to obtain compound III as a yellow colloidal solid (245.7mg, 71%) .
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