反应 #1089625
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03984501
反应条件: temp:210.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To 4.3 g (0.0136 mole) of 1-(4-methoxyphenyl)-2-benzyl-3-phenylpropane was added 4 g (0.0346 mole) of pyridine hydrochloride and heated to 210°C for 5 hours. The mixture was cooled, and 300 ml H2O and 300 ml chloroform were added. Chloroform layer was separated, washed with 4 × 250 ml H2O and dried over anhydrous MgSO4. Chloroform was removed at reduced pressure. The residue was distilled at 210°-215°C/0.3 mm. Yield 3.5 g (85.16%). This material can also be obtained by alkylation of 1-phenyl-3-(4-methoxyphenyl)-1-propanone or 1-(4-methoxyphenyl)-3-phenyl-1-propanone with α-chlorotoluene as carried out in Example I, followed by demethylation with pyridine hydrochloride and reduction of the carbonyl function. The mixture was cooled Chloroform layer was separated washed with 4 × 250 ml H2O dried over anhydrous MgSO4 Chloroform was removed at reduced pressure The residue was distilled at 210°-215°C/0.3 mm
来源 ID: ord-f2e344ab649f4b388033da756012b183