تفاعل #342076

ord-0aca38ac87b54e4996621794bc5a5aad

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture was reacted at room temperature for 2 hours
  2. 2
    درجة الحرارةwith gradual increase of temperature
  3. 3
    تركيزThe reaction mixture was concentrated
  4. 4
    أخرىdried in a vacuum
  5. 5
    أخرىThe residue was purified through alumina column (ICN Biomedicals. GmbH, ICN Alumina N, Act.1/eluent acetonitrile)
  6. 6
    تركيزThe eluate was concentrated
  7. 7
    أخرىdried in a vacuum

الإجراء التجريبي

In 116 g of dehydrated chloroform (reagent, Wako Pure Chemical Ind. Ltd.) was dissolved 24.3 g of N-methoxymethyl-N-methylpyrrolidinium chloride. To the solution was added dropwise 24.3 g of trifluoromethane sulfonic acid (reagent, Aldrich Corp.) at 5° C. over a period of 1 hour. The mixture was reacted at room temperature for 2 hours with gradual increase of temperature. The reaction mixture was concentrated and dried in a vacuum. The residue was purified through alumina column (ICN Biomedicals. GmbH, ICN Alumina N, Act.1/eluent acetonitrile). The eluate was concentrated and dried in a vacuum to obtain 39.1 g of the desired product (colorless liquid).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07875732B2uspto-grants-2011_01