تفاعل #440651

ord-24866de84850439da6e781961c2fdce3

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزAfter a night at room temperature the solution is concentrated to dryness by distillation under reduced pressure
  2. 2
    أخرىthe resulting residue is purified by flash chromatography (silica gel, 200 g; eluent CH2Cl2/MeOH/TEA 15/5/02)

الإجراء التجريبي

A solution of ethyl 4-chloroacetoacetate (7.02 ml) and ammonium acetate (11.8 g) in absolute ethanol (180 ml) is refluxed for 3 hours. After a night at room temperature the solution is concentrated to dryness by distillation under reduced pressure and the resulting residue is purified by flash chromatography (silica gel, 200 g; eluent CH2Cl2/MeOH/TEA 15/5/02), to give 6.53 g of ethyl (Z)-3-amino-4-chloro-2-butenoate as dark oil which is used without further purifications.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06753342B2uspto-grants-2004_06