Реакция #158271

ord-5a0c6204eb8d498e8a613db833cb2c94

Растворители

Условия реакции

Температура
-10°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for 16 hr
  2. 2
    ДругоеThe solvent in the reaction mixture was evaporated under reduced pressure, and water
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    ФильтрацияThe resultant solid was collected by filtration
  5. 5
    Промывкаwashed with water
  6. 6
    Другоеdried under reduced pressure
  7. 7
    Промывкаwashed with IPE

Методика

N,N′-Carbonyldiimidazole (115 g) was added to a suspension of 3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzoic acid (83.0 g) in THF (1 L) at room temperature, and the mixture was stirred for 1 hr. The reaction mixture was cooled to −10° C., hydrazine monohydrate (173 mL) was added, and the mixture was stirred at room temperature for 16 hr. The solvent in the reaction mixture was evaporated under reduced pressure, and water was added to the residue. The resultant solid was collected by filtration, washed with water, dried under reduced pressure, and washed with IPE to give the title compound (85.8 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822699B2uspto-grants-2014_09