Preparation method for (1S)-1,6-dideoxy-1-[4-hydroxy-3-(trans-4-substituted cyclohexyl) methyl phenyl]-D-glucopyranose compound
A compound and deacetylation technology, applied in the field of medicine, can solve the problems of relatively large yield fluctuation, low overall route yield, poor route reproducibility, etc.
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[0047] [1]
[0048]
[0049] Add 32.52g (0.1mol) compound XIV-1, 20.52g (0.12mol) benzyl bromide, 27.64g (0.2mol) solid K in a dry 500mL round bottom flask 2 CO 3 , 5.00 g of solid KI and 200 mL of dry DMF, the resulting mixture was stirred at room temperature overnight, TLC showed that the reaction was complete.
[0050] The reaction mixture was washed with 500 mL CH 2 Cl 2 Dilute, stir for 1 minute, and filter with suction to remove solids. The filtrate was washed with saturated brine, anhydrous Na 2 SO 4 After drying, the desiccant was removed by suction filtration, and the solvent was evaporated in a rotary evaporator to obtain a colorless oil, which was purified by column chromatography to obtain the pure product XIII-1, 37.80 g, with a yield of 91%. Colorless crystals, melting point 63-65°C, 1 H NMR (DMSO-d 6 ,400MHz),δ7.67(dd,1H,J=2.4Hzand8.8Hz),7.53(d,1H,J=2.8Hz),7.35-7.49(m,5H),7.25(d,1H,J=8.8 Hz),5.19(s,2H),3.01-3.08(m,1H),1.71-1.74(m,2H),1.59-1.63(m,2H)...
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