Reaktion #730368

ord-2577b84cc177486b9b1012e05d9563ea

Reaktionsgleichung

CCN(C)CC
N,N diethyl-N-methvlamine
COCCl
chloromethyl methyl ether
CC[N+](C)(CC)COC.[Cl-]
desired product
CC[N+](C)(CC)COC.[Cl-]
N,N-diethyl-N-methyl-N-methoxymethylammonium Chloride

Lösungsmittel

Reaktionsbedingungen

Temperatur
5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated to a gradually elevated temperature
  2. 2
    workup.STIRRINGstirred at room temperature for 10 hours
  3. 3
    Sonstigethe reaction
  4. 4
    FiltrationThe reaction mixture was filtered
  5. 5
    Sonstigethe solids obtained
  6. 6
    Waschenwere washed with 150 g of toluene and 150 g of acetone
  7. 7
    Sonstigedried in a vacuum

Vorschrift

A 30.0 g quantity of N,N diethyl-N-methvlamine (reagent, product of Tokyo Kasei Co., Ltd.) was dissolved in 120 g of toluene, followed by nitrogen replacement. Over a period of 1 hour, 31.2 g of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd.) was added dropwise to the solution at 5° C. The mixture was stirred at 5° C. for 1 hour, heated to a gradually elevated temperature and stirred at room temperature for 10 hours to complete the reaction. The reaction mixture was filtered, and the solids obtained were washed with 150 g of toluene and 150 g of acetone and then dried in a vacuum, giving 53.7 g of the desired product (white solid).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07700243B2uspto-grants-2010_04