تفاعل #169541

ord-ec39c84d5e1f4e72b64dbc6f9ace4b66

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةUpon cooling to room temperature
  2. 2
    تركيزthe mixture was concentrated in vacuo
  3. 3
    غسيلrinsed with hexane

الإجراء التجريبي

4-Chloro-3-fluorobenzaldehyde (1.0 g, 6.3 mmol) was added to a solution of ethyl 2-cyanoacetate (0.71 g, 6.3 mmol) and piperidine (0.081 ml, 0.82 mmol) in toluene (10 mL) at room temperature. The mixture was heated at 100° C. for 7 hours. Upon cooling to room temperature, the mixture was concentrated in vacuo and rinsed with hexane to give ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanoacrylate (1.4 g, 88%). LCMS (APCI+) [M+H]+253.1.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846681B2uspto-grants-2014_09