تفاعل #56425

ord-bd0f204d655b49bc89bebaccd7c04c7b

معادلة التفاعل

CC(C)Br
2-bromopropane
O=C(Cc1ccccc1)N(c1ccc(Cl)cc1)C1CCNCC1
N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
[I-].[K+]
potassium iodide
CC(C)Br
2-bromopropane
CC(C)N1CCC(N(C(=O)Cc2ccccc2)c2ccc(Cl)cc2)CC1.Cl
N-(4-chlorophenyl)-N-[1-(1-methylethyl)-4-piperidinyl]benzeneacetamide hydrochloride

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    درجة الحرارةrefluxed for 20 hours
  3. 3
    workup.STIRRINGstirring
  4. 4
    درجة الحرارةrefluxing
  5. 5
    درجة الحرارةThe reaction mixture is cooled
  6. 6
    ترشيحfiltered
  7. 7
    أخرىthe filtrate is evaporated
  8. 8
    ترشيحThe precipitated solid salt is filtered off
  9. 9
    أخرىcrystallized from a mixture of 2-propanone and 2-propanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04225606uspto-grants-1980_09