Reacción #45034

ord-f84d078d214a4f8796164fe9bb277e0c

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe reaction mixture was separated
  2. 2
    Lavadothe organic layer was washed with water (2×15 ml) and brine (2×15 ml)
  3. 3
    Secadodried over sodium sulphate
  4. 4
    Filtraciónfiltered
  5. 5
    Otroevaporated
  6. 6
    Otrodried in vacuo

Procedimiento

Potassium hydroxide (11.19 g, 199.4 mmol) dissolved in water (44.8 ml) was added to a solution of 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine (7.121 g) dissolved in dichloromethane (40 ml). A solution of (2-methylpropan-2-yl)oxycarbonyl tert-butyl carbonate (6.8 g, 31.2 mmol) in DCM (35 ml) was added and the reaction mixture was stirred vigorously at room temperature for 4 h. The reaction mixture was separated and the organic layer was washed with water (2×15 ml) and brine (2×15 ml), dried over sodium sulphate, filtered, evaporated and dried in vacuo to give tert-butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate (8.70 g, 99%) as a cream solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07737149B2uspto-grants-2010_06