반응 #56425
ord-bd0f204d655b49bc89bebaccd7c04c7b
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시약
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후처리
- 1workup.ADDITIONAfter the addition
- 2온도refluxed for 20 hours
- 3workup.STIRRINGstirring
- 4온도refluxing
- 5온도The reaction mixture is cooled
- 6여과filtered
- 7기타the filtrate is evaporated
- 8여과The precipitated solid salt is filtered off
- 9기타crystallized from a mixture of 2-propanone and 2-propanol
실험 절차
To a stirred suspension of 5 parts of N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, a few crystals of potassium iodide in 200 parts of butanol is added dropwise 4 parts of 2-bromopropane at room temperature. After the addition is complete, the whole is stirred and refluxed for 20 hours. Then the second portion of 4 parts of 2-bromopropane is added and stirring and refluxing is continued for another 19 hours. The reaction mixture is cooled, filtered and the filtrate is evaporated. From the oily free base, the hydrochloride salt is prepared in the conventional manner in 1,1'-oxybisethane and 2-propanone. The precipitated solid salt is filtered off and crystallized from a mixture of 2-propanone and 2-propanol, yielding 2 parts of N-(4-chlorophenyl)-N-[1-(1-methylethyl)-4-piperidinyl]benzeneacetamide hydrochloride; mp. 263° C.