Реакция #58623

ord-ef5a843594ce4bdbbd44b4fce50222a8

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    ДругоеThe solvent was evaporated under vaccum
  3. 3
    Другоеthe residue was triturated with H2O

Методика

To a stirred solution of methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate (1 eq) in glacial acetic acid (20 mL) was added a solution of bromine (1.3 eq) in glacial acetic acid (5 mL) slowly over a period of 5 min. After the addition was complete, the resulting dark solution was stirred for 30 mins at RT. The solvent was evaporated under vaccum and the residue was triturated with H2O. The title compound was obtained by filtration (99%) as an off-white solid. The product was used in the next step without any further purification after drying for 2 days under P2O5. LC/MS (ES, M+H=425).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07423061B2uspto-grants-2008_09