Réaction #2132864

ord-0bf0635cb0bc4e82b2f5209bef3516a3

Équation de réaction

CCCC[n+]1ccn(C)c1.[Cl-]
1-butyl-3-methylimidazolium chloride
[Na+].[OH-]
NaOH
CCCC[n+]1ccn(C)c1.[Cl-]
1-butyl-3-methylimidazolium chloride
CCCC[n+]1ccn(C)c1.[OH-]
1-butyl-3-methylimidazolium hydroxide

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas poured
  2. 2
    workup.ADDITIONthis mixture was poured into the activated Amberlite IRA400 (OH)

Mode opératoire

Amberlite IRA400 (OH) (140 mL) was poured into a chromatographic column tube, and 1N NaOH aqueous solution (2.5 L) was poured therein to activate the Amberlite IRA400 (OH). Thereafter, pure water (1.5 L) was poured into the tube until a filtrate became neutral. Pure water (50 mL) was added to 1-butyl-3-methylimidazolium chloride (5.0 g, 28.63 mmol) to melt the 1-butyl-3-methylimidazolium chloride, and this mixture was poured into the activated Amberlite IRA400 (OH), to obtain a 1-butyl-3-methylimidazolium hydroxide aqueous solution. Pure water (200 mL) and THF (100 mL) was added to phenylacetate (3.9 g, 28.63 mmol) and was made into an even solution. Into this solution, the 1-butyl-3-methylimidazolium hydroxide aqueous solution was slowly dropped, and the mixture was stirred at 0° C. for 12 hours. A reaction solution was concentrated; acetonitrile (90 mL) and methanol (10 mL) were added to an obtained residue, and the mixture was stirred at 0° C. for 30 minutes. A filtrate was concentrated, and was dried by heat under reduced pressure to obtain 8.0 g of an object compound as a light yellow oily matter. (100% yield)

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08591757B2uspto-grants-2013_11