反应 #2830097
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04039685
反应条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5.7 gm (0.02 mol) of 1-(2-cyanophenoxy)-2-hydroxy-3-tert.-butylamino propane (prepared analogous to Example II) were dissolved in 32 ml of concentrated HCl and while stirring at 45° C. 2.27 gm of 35% hydrogen peroxide were added drowise so that the temperature did not exceed 65° C. Thereafter, the temperature was maintained at 60° C. for 30 minutes and the mixture was concentrated in vacuo at the end of which a solid residue remained. The raw hydrochloride was recrystallized from ethanol under an addition of ether to obtain 3 gm of 1-(2-cyano-4-chloro-phenoxy)-2-hydroxy-3-tert.-butylamino propane hydrochloric having a melting point of 180°-182° C. did not exceed 65° C Thereafter, the temperature was maintained at 60° C. for 30 minutes the mixture was concentrated in vacuo at the end of which a solid residue The raw hydrochloride was recrystallized from ethanol under an addition of ether
来源 ID: ord-124b2705867f46f4a69a003790a62dd0