Reacción #46899

ord-11b7e1b587b24149a996c26f3b6cd29a

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe organic solvent was evaporated
  2. 2
    FiltraciónThe formed crystalline material was filtered off
  3. 3
    workup.ADDITIONtreated once with about 50 mL of a saturated NaHCO3-solution under ultrasonic conditions
  4. 4
    FiltraciónThe crystalline residue was filtered off again
  5. 5
    Lavadowashed twice with 20 mL water
  6. 6
    OtroDrying under reduced pressure at 35° C.

Procedimiento

A solution of 500.0 mg (1.85 mmol) 5-Chloro-2-trichloromethyl-1H-benzoimidazole in 20 mL THF was added slowly to a mixture of 286 μl (2.04 mmol) diisopropyl-amine and 1.55 g (18.5 mmol, 10 equivalents) NaHCO3 in 70 mL THF and 20 mL water. The reaction mixture was stirred for 2 h at RT. The organic solvent was evaporated. The formed crystalline material was filtered off and treated once with about 50 mL of a saturated NaHCO3-solution under ultrasonic conditions. The crystalline residue was filtered off again and washed twice with 20 mL water. Drying under reduced pressure at 35° C. gave pure 5-Chloro-1H-benzoimidazole-2-carboxylic acid diisopropylamide in form of a light brown crystalline solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07741341B2uspto-grants-2010_06