Reaktion #470363

ord-93e7d5f749554c77be7bdbb8b0293c89

Reaktionsgleichung

CN1CCCC1
N-methylpyrrolidine
COCBr
bromomethyl methyl ether
COC[N+]1(C)CCCC1.[Br-]
desired product
COC[N+]1(C)CCCC1.[Br-]
N-Methoxymethyl-N-Methylpyrrolidinium Bromide

Lösungsmittel

Reaktionsbedingungen

Temperatur
15°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto terminate
  2. 2
    Sonstigethe reaction
  3. 3
    FiltrationThe reaction mixture was filtered
  4. 4
    Waschenthe resulting solids were washed with 160 g of acetone
  5. 5
    Sonstigedried in a vacuum

Vorschrift

A 17.0 g quantity of N-methylpyrrolidine was dissolved in 160 g of dehydrated acetone (up to 0.1% in water content), followed by nitrogen replacement. To the solution was added dropwise 24.6 g of bromomethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd.) at 5° C. over a period of 1.5 hours. The mixture was stirred at 5 to not higher than 15° C. for 4 hours to terminate the reaction. The reaction mixture was filtered, and the resulting solids were washed with 160 g of acetone, and dried in a vacuum, affording 30.9 g of the desired product (white solid).

Quelle

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