تفاعل #440651
ord-24866de84850439da6e781961c2fdce3
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزAfter a night at room temperature the solution is concentrated to dryness by distillation under reduced pressure
- 2أخرىthe 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.