Reaktion #470375

ord-9209a896dfa1435f880b571e2d41bd2d

Reaktionsgleichung

CC(C)N1CCCC1
N-isopropylpyrrolidine
COCCl
chloromethyl methyl ether
COC[N+]1(C(C)C)CCCC1.[Cl-]
desired product
COC[N+]1(C(C)C)CCCC1.[Cl-]
N-Methoxymethyl-N-Isopropylpyrrolidinium Chloride

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was thereafter heated to a gradually elevated temperature
  2. 2
    Sonstigewhereby the reaction was terminated
  3. 3
    TemperaturThe reaction mixture was cooled to 5° C.
  4. 4
    Filtrationthe resulting solids were filtered off in nitrogen
  5. 5
    WaschenThe filter cake was washed with 200 ml of 2-butanone
  6. 6
    Sonstigedried in a vacuum

Vorschrift

A 40.00 g quantity of N-isopropylpyrrolidine was dissolved in 361 g of dehydrated 2-butanone (reagent, product of Wako Pure Chemical Ind. Ltd.), followed by replacement with nitrogen. To the solution was added dropwise 28.76 g of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd. as purified by distillation) at 5° C. over a period of 0.5 hour. The mixture was thereafter heated to a gradually elevated temperature and stirred at room temperature for 10 hours, whereby the reaction was terminated. The reaction mixture was cooled to 5° C., and the resulting solids were filtered off in nitrogen. The filter cake was washed with 200 ml of 2-butanone and thereafter dried in a vacuum, giving 66.40 g of the desired product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08366956B2uspto-grants-2013_02