反应 #1320801
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05204343
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 15.64 g (73.6 mmoles) of dl-3-(3,4-dimethoxyphenyl)-propane-1,2-diol (II) are dissolved in 200 ml of benzene. 8.03 ml (73.6 mmoles) of 3-chlorobenzaldehyde and 4.6 ml (56 mmoles) of concentrated hydrochloric acid are added to the solution and the reaction mixture is stirred for 5 hours at room temperature. The solution is then evaporated in vacuo, the oily residue is dissolved in 200 ml of 99.5% ethanol, clarified while hot, filtered and the filtrate is evaporated in vacuo. Thus 23.19 g (94%) of crude product are obtained in oily form, which can be used for the further reaction steps without purification (the purity of the product exceeds 95%). The solution is then evaporated in vacuo the oily residue is dissolved in 200 ml of 99.5% ethanol filtered the filtrate is evaporated in vacuo
来源 ID: ord-fe4e541c470a43f0a67efe2cc0c633b5