반응 #65986

ord-4e1d8e28a6e24573986f57e5613b61a1

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe reaction mixture is stirred for 90 minutes at -8° to 10° C
  2. 2
    workup.STIRRINGstirred for i hour at 0° C
  3. 3
    기타The reaction mixture is removed from the ice bath
  4. 4
    workup.STIRRINGis stirred at room temperature for 20 hours
  5. 5
    여과The mixture is then filtered
  6. 6
    세척washed with water

실험 절차

A solution of sodium nitrite (3.8 g, 0.055 mol in 20 mL of H2O), is added dropwise to an ice cold stirring suspension of 4-benzyloxyaniline (13.0 g, 0.055 mol in 150 mL of concentrated HCl). The reaction mixture is stirred for 90 minutes at -8° to 10° C. A solution of SnCl2 ·2H2O (32.0 g, 0142 mol in 50 mL concentrated HCl) is added and stirred for i hour at 0° C. The reaction mixture is removed from the ice bath and is stirred at room temperature for 20 hours. The mixture is then filtered and washed with water to give 13.0 g (95% yield) of product, m.p. 182°-185° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420289uspto-grants-1995_05