反応 #470364

ord-143614ae0ca4455dacc462476a3cf9db

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The mixture was reacted at room temperature for 0.5 hour
  2. 2
    その他whereby the reaction was terminated
  3. 3
    濃縮The reaction mixture was concentrated
  4. 4
    乾燥dried in vacuum, and 100 ml of ethyl alcohol
  5. 5
    workup.ADDITIONwas added to the residue
  6. 6
    その他to remove insoluble sodium chloride
  7. 7
    workup.DISSOLUTIONThe resulting product was dissolved in dichloromethane
  8. 8
    ろ過the solution was filtered with a membrane
  9. 9
    ろ過filter again
  10. 10
    濃縮the filtrate was concentrated in a vacuum
  11. 11
    その他dried

実験手順

A 1.60 g quantity of sodium carbonate (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 18 g of deionized water, and 5.01 g of N-methoxymethyl-N-methylpyrrolidinium chloride was added to the solution. The mixture was reacted at room temperature for 0.5 hour, whereby the reaction was terminated. The reaction mixture was concentrated and dried in vacuum, and 100 ml of ethyl alcohol was added to the residue to remove insoluble sodium chloride. The resulting product was dissolved in dichloromethane, the solution was filtered with a membrane filter again, and the filtrate was concentrated in a vacuum and dried, giving 5.41 g of the desired product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08366956B2uspto-grants-2013_02