反应 #1619563
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04217350
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The 1-[2-hydroxy-3-(2-methoxyphenyloxy)-propyl]-4-[2-(4-chloroanilino)-ethylamino]-piperidine can be prepared as follows: A mixture of 38 g of p-chloroaniline and 31 g of 2-bromoethylamine-hydrobromide is heated to 70° C. with stirring. After 30 minutes 75 ml of diethyl ketone are added and the mixture is refluxed for 4 hours. The black solution is then concentrated under reduced pressure. The residue is made alkaline with 2 N sodium carbonate solution and extracted with three 100 ml portions of chloroform. The residual oil is fractionally distilled in vacuo to yield 1-(4-chlorophenyl)-ethylenediamine with a boiling point of 130°-135° C. (1.5 torr). the mixture is refluxed for 4 hours The black solution is then concentrated under reduced pressure extracted with three 100 ml portions of chloroform The residual oil is fractionally distilled in vacuo
来源 ID: ord-0a6dd3ebc6f145e2bf583a446512c9c6