تفاعل #470366

ord-96ecff76950647ebafe1a913cd6feca8

معادلة التفاعل

[F-].[K+]
potassium fluoride
COC[N+]1(C)CCCC1.[O-][Cl+3]([O-])([O-])[O-]
N-methoxymethyl-N-methylpyrrolidinium perchlorate
COC[N+]1(C)CCCC1.[F-]
desired product
COC[N+]1(C)CCCC1.[F-]
N-Methoxymethyl-N-Methylpyrrolidinium Fluoride

الكواشف

لا شيء

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
    workup.ADDITIONWith addition of 100 ml of methanol
  4. 4
    ترشيحthe reaction mixture was filtered
  5. 5
    تركيزThe filtrate was concentrated
  6. 6
    أخرىdried in a vacuum
  7. 7
    workup.DISSOLUTIONThe residue was then dissolved in dichloromethane
  8. 8
    ترشيحthe solution was again filtered with a membrane
  9. 9
    ترشيحfilter
  10. 10
    تركيزthe filtrate was concentrated
  11. 11
    أخرىdried

الإجراء التجريبي

A 0.44 g quantity of potassium fluoride (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 11 g of deionized water, and 1.74 g of N-methoxymethyl-N-methylpyrrolidinium perchlorate was added to the solution. The mixture was reacted at room temperature for 1.5 hours, whereby the reaction was terminated. With addition of 100 ml of methanol, the reaction mixture was filtered. The filtrate was concentrated and dried in a vacuum. The residue was then dissolved in dichloromethane, the solution was again filtered with a membrane filter, and the filtrate was concentrated and dried, giving 1.05 g of the desired product.

المصدر

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