تفاعل #470368

ord-00abe886f9844638b8294a0e97662f94

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    أخرىwhereby the reaction was terminated
  3. 3
    ترشيحThe reaction mixture was filtered
  4. 4
    تركيزthe filtrate was concentrated
  5. 5
    أخرىdried in a vacuum
  6. 6
    workup.ADDITIONTo the residue was added 100 ml of dichloromethane
  7. 7
    ترشيحfollowed by filtration with a membrane
  8. 8
    ترشيحfilter
  9. 9
    تركيزconcentration in a vacuum
  10. 10
    أخرىdrying

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08366956B2uspto-grants-2013_02