반응 #78478

ord-155db5bb947b455ebd5997a0332e3da3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITAfter 2 hours at 60° C.
  2. 2
    workup.DISTILLATIONthe solvent was distilled off
  3. 3
    workup.ADDITIONthe crystalline residue was mixed with water
  4. 4
    세척washed with water
  5. 5
    기타dried
  6. 6
    기타After crystallization from ethanol
  7. 7
    기타9.95 g (91% of theory) were obtained in the form of white crystals

실험 절차

11.4 g (63 mmol) of 4-cyanophenoxyacetic acid were dissolved in 200 mL of absolute tetrahydrofuran and mixed at room temperature with 10.2 g (63 mmol) of N,N′-carbonyldiimidazole. After 15 minutes at 60° C., 5.70 g (41.5 mmol) of 2-amino-3-methylamino-6-methylpyridine were added. After 2 hours at 60° C., the solvent was distilled off and the crystalline residue was mixed with water, washed with water, and dried. After crystallization from ethanol, 9.95 g (91% of theory) were obtained in the form of white crystals. C16H14N4O (278.32). Mass spectrum: M+=278.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710055B2uspto-grants-2004_03