Réaction #685004

ord-7f0db751eea642768439a80fa868c622

Équation de réaction

Cl
hydrogen chloride
CN(C)C1CCN(CCCOCCc2ccc3sccc3c2)C1
1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-N,N-dimethyl-3-pyrrolidinamine
CN(C)C1CCN(CCCOCCc2ccc3sccc3c2)C1.Cl.Cl
achromatic crystal
CN(C)C1CCN(CCCOCCc2ccc3sccc3c2)C1.Cl.Cl
1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-N,N-dimethyl-3-pyrrolidinamine dihydrochloride

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas added to the obtained solution
  2. 2
    workup.WAITat 5° C. for 1 hour
  3. 3
    AutreThereafter, precipitated crystals
  4. 4
    Filtrationwere collected by filtration
  5. 5
    LavageThe crystals were washed with ethyl acetate
  6. 6
    Autredried

Mode opératoire

0.39 g of 1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-N,N-dimethyl-3-pyrrolidinamine was dissolved in 4.0 ml of ethyl acetate. Thereafter, 0.80 ml of an ethyl acetate solution containing 3.25 mol/l dry hydrogen chloride was added to the obtained solution, and the mixture was stirred at a room temperature for 1 hour and then at 5° C. for 1 hour. Thereafter, precipitated crystals were collected by filtration. The crystals were washed with ethyl acetate and then dried, so as to obtain 0.32 g of an achromatic crystal, 1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-N,N-dimethyl-3-pyrrolidinamine dihydrochloride.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07897594B2uspto-grants-2011_03