Reacción #6910

ord-410a6f1443c34331ba6735f7cc64c911

Condiciones de reacción

Temperatura
90°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Lavadowashed twice with brine
  2. 2
    Secadodried over sodium sulfate
  3. 3
    Filtraciónfiltered through a fritted funnel
  4. 4
    Otrothe volatiles were removed under vacuum
  5. 5
    OtroThis provided the product, MS
  6. 6
    Otrom/z 356, which was used in the next step without further purification

Procedimiento

A mixture of the product of Step D (60 mg; 0.1863 mmol), hydroxyl amine hydrochloride (3 eq.), sodium carbonate (4 eq.) in 1.5 mL water and 2.5 mL ethanol was heated to 90° C. for 6 h. The mixture was diluted with dichloromethane, washed twice with brine, dried over sodium sulfate, filtered through a fritted funnel and the volatiles were removed under vacuum. This provided the product, MS: m/z 356, which was used in the next step without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07084156B2uspto-grants-2006_08