Реакция #470368

ord-00abe886f9844638b8294a0e97662f94

Уравнение реакции

CC(=O)[O-].[Na+]
sodium acetate
COC[N+]1(C)CCCC1.[Cl-]
N-methoxymethyl-N-methylpyrrolidinium chloride
COC[N+]1(C)CCCC1.[Cl-]
N-Methyl-N-Methoxymethylpyrrolidinium Chloride
CC(=O)[O-].COC[N+]1(C)CCCC1
desired product
CC(=O)[O-].COC[N+]1(C)CCCC1
N-Methoxymethyl-N-Methylpyrrolidinium Acetate

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    Другоеwhereby the reaction was terminated
  3. 3
    ФильтрацияThe reaction mixture was filtered
  4. 4
    Концентрированиеthe filtrate was concentrated
  5. 5
    Другоеdried in a vacuum
  6. 6
    workup.ADDITIONTo the residue was added 100 ml of dichloromethane
  7. 7
    Фильтрацияfollowed by filtration with a membrane
  8. 8
    Фильтрацияfilter
  9. 9
    Концентрированиеconcentration in a vacuum
  10. 10
    Другоеdrying

Методика

A 9.46 g quantity of sodium acetate (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 95 g of methanol, and 19.10 g of N-methoxymethyl-N-methylpyrrolidinium chloride was added to the solution. The mixture was reacted at room temperature for 1.5 hours, whereby the reaction was terminated. The reaction mixture was filtered, and the filtrate was concentrated and dried in a vacuum. To the residue was added 100 ml of dichloromethane, followed by filtration with a membrane filter, concentration in a vacuum and drying, affording 20.38 g of the desired product.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08366956B2uspto-grants-2013_02