تفاعل #70456

ord-027bcfb2f02b474e89a07d6e5c810596

الكواشف

لا شيء

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    تركيزThe reaction mixture is concentrated
  2. 2
    workup.ADDITIONEtOAc (50 mL) and water (15 mL) are added
  3. 3
    غسيلThe organic fraction washed with water
  4. 4
    تجفيفbrine, then is dried over sodium sulfate
  5. 5
    أخرىThe solvent is evaporated under reduced pressure

الإجراء التجريبي

Solid Na2CO3 (400 mg, 3.8 mmol, 3.8 eq) is added to a solution of 1-benzyl-4-chlorophthalazine (250 mg, 0.98 mmol, 1 eq) and (5)-2-methyl-piperazine (400 mg, 4.0 mmol, 4.0 eq) in dioxane (5 mL). The resulting suspension is heated at 100° C. for 48 h. The reaction mixture is concentrated, EtOAc (50 mL) and water (15 mL) are added. The organic fraction washed with water and then brine, then is dried over sodium sulfate. The solvent is evaporated under reduced pressure to afford the title compound as a white solid (200 mg, 64% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536168B2uspto-grants-2013_09