تفاعل #411173

ord-0b6a35b019f04d9495b454e5f4a67756

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGwith stirring
  2. 2
    workup.STIRRINGThe mixture was stirred at ambient temperature for 2 hours
  3. 3
    أخرىthe ethanol removed under reduced pressure
  4. 4
    workup.ADDITIONIce cold 2M hydrochloric acid (400 ml) was added to the residue
  5. 5
    غسيلthe mixture was washed with ether
  6. 6
    استخلاصextracted with dichloromethane

الإجراء التجريبي

Diethyl malonate (52.45 g) in ethanol (50 ml) was added dropwise to a solution of sodium (11.3 g) in dry ethanol (300 ml) with stirring. The mixture was cooled to 0° C. and a solution of 1-benzyl-2-chloromethylimidazole hydrochloride (40.0 g, prepared as described in J.A.C.S. 1949, 383) in dry ethanol (250 ml) was added over 30 minutes with stirring. The mixture was stirred at ambient temperature for 2 hours and then the ethanol removed under reduced pressure. Ice cold 2M hydrochloric acid (400 ml) was added to the residue and the mixture was washed with ether. The aqueous layer was basified with solid sodium carbonate and then extracted with dichloromethane to give ethyl 2-carbethoxy-3-(1-benzyl-1H-imidazol-2-yl)propanoate as an oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06215001B1uspto-grants-2001_04