تفاعل #71323

ord-772ab5a6080a4b2ab56013fb6350e3ff

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
180°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool to rt
  2. 2
    ترشيحfiltered

الإجراء التجريبي

A mixture of 5-bromo-8-(3,5-dimethoxy-phenyl)-quinoxaline (Step 1.4) (4.54 g, 13.2 mmol) and CuCN (1.54 g, 17.1 mmol, 1.3 equiv) in NMP (50 mL) was stirred for 2 h at 180° C., under an argon atmosphere. The reaction mixture was allowed to cool to rt, diluted with EtOAc (10% aqueous solution of ethylenediamine) (150 mL), and filtered to afford 1.19 g (batch 1) of the title compound as a yellow solid. The filtrate was extracted with DCM. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated in EtOAc to provide 2.31 g (batch 2) of the title compound: ESI-MS: 292.1 [M+H]+; tR=4.53 min (System 1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536175B2uspto-grants-2013_09