反应 #3078693
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04075238
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: When the procedure of Example 64 was carried by replacing tetrachloro-p-xylene with an equimolar amount (27.6g) of 2,3,5,6-tetrachloro-p-xylene-α ,α'-diol, a strong evolution of sulfur dioxide was observed (identified qualitatively by iodine paper), but the resultant solution did not turn purple, instead it acquired a brown amber color. After a 4 hour of heating period between 90° and 94° C, the clear solution was poured, after it cooled to room temperature, onto ice, yielding a yellow slurry. Since filtration was sluggish, the slurry was extracted with diethyl ether, yielding, after evaporation of the solvent 19.0 g of bright yellow solids, whose identity was determined by infrared and nuclear magnetic resonance spectra, which matched those described in Example 64. After a 4 hour of heating period between 90° and 94° C the clear solution was poured yielding a yellow slurry Since filtration the slurry was extracted with diethyl ether yielding after evaporation of the solvent 19.0 g of bright yellow solids, whose identity
来源 ID: ord-f0157582cbb3480aa527d75ea592912c