تفاعل #1132923

ord-0b741a4e7c41437fb51529d8cc3eea1f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe resulting mixture was heated
  2. 2
    درجة الحرارةat reflux overnight
  3. 3
    أخرىthe solvent was evaporated
  4. 4
    workup.ADDITIONThe residue was mixed with saturated aqueous NaHCO3 (100 mL)
  5. 5
    استخلاصextracted with CH2Cl2 (100 mL×3)
  6. 6
    تجفيفThe combined organic layers were dried over anhydrous Na2SO4
  7. 7
    تركيزconcentrated in vacuo
  8. 8
    أخرىThe residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2

الإجراء التجريبي

A 250 mL round bottom flask was charged with 2-chloro-6-methylpyrazine (4.0 g, 0.031 mol), 1-methylpiperazine (12.4 g, 0.125 mol) and EtOH (100 mL). The resulting mixture was heated at reflux overnight. Work-up: the solvent was evaporated. The residue was mixed with saturated aqueous NaHCO3 (100 mL) and then extracted with CH2Cl2 (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2, to afford 2.7 g (45%) of the product as a white solid. MS m/z: 193 (M+H+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08569300B2uspto-grants-2013_10