Reacción #216159

ord-bf33a29f5886453aae83781a0538dfb4

Disolventes

Condiciones de reacción

Temperatura
-5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRING' stirring at room temperature
  2. 2
    OtroThe solution was evaporated in vacuo
  3. 3
    Otrothe residue triturated with ether

Procedimiento

The product from step (b) (10.3 g) was suspended in water (53 ml) and c.HCl (106 ml) added dropwise. The resulting mixture was cooled to -5° C. and a solution of sodium nitrite (3.2 g) in water (30 ml) added dropwise to the stirred mixture over 15 minutes followed by 30 minutes' stirring at -5° to 0° C. The solution was then added at 0° C. over 15 minutes to a stirred solution of tin (II) chloride (51 g) in c.HCl (91 ml), followed by 3 hours' stirring at room temperature. The solution was evaporated in vacuo and the residue triturated with ether to give the desired product as a pale yellow solid (11 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05466699uspto-grants-1995_11