تفاعل #71332

ord-2f385962300641b9b2684ff96426fc9e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe aqueous layer was separated
  2. 2
    استخلاصextracted with DCM
  3. 3
    غسيلThe organic phase was washed with H2O and brine
  4. 4
    تجفيفdried (Na2SO4)
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated
  7. 7
    أخرىThe residue was triturated in Et2O

الإجراء التجريبي

A mixture of 4-(4-{[8-(2,6-dichloro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonyl]-amino}-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (Step 8.1) (137 mg, 0.22 mmol) and a 4 N solution of HCl in dioxane (5 mL) was stirred for 1 h at rt. The reaction mixture was diluted with DCM and H2O. The aqueous layer was separated and extracted with DCM. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated in Et2O to afford 95 mg of the title compound as a red solid: ESI-MS: 537.9/539.9 [M+H]+; tR=4.01 min (System 1).

المصدر

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