Reacción #1463490

ord-efb5e4f2969d495b8879ca73d5266dad

Ecuación de reacción

BrBr
bromine
BrBr
bromine
O
water
O=S([O-])[O-].[Na+].[Na+]
sodium sulfite
BrBr
bromine
CCC(CC)Nc1cccc2c1C(=O)c1ccccc1C2=O
EPAQ
CCC(CC)Nc1cccc2c1C(=O)c1ccccc1C2=O
1-(1-ethylpropylamino)anthraquinone
CCC(CC)Nc1ccc(Br)c2c1C(=O)c1ccccc1C2=O
1-(1-ethylpropylamino)-4-bromoanthraquinone

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added
  2. 2
    OtroThe aqueous solution was decanted off
  3. 3
    workup.DISSOLUTIONThe solid was dissolved in methylene chloride
  4. 4
    Concentraciónconcentrated
  5. 5
    workup.ADDITIONslowly added to cold methanol, whereupon a solid
  6. 6
    Otroprecipitated

Procedimiento

EPAQ (20.02 g) was dissolved in hot acetic acid. In a separate flask, bromine (12.03 g) was dissolved in acetic acid (ca. 10 mL). The bromine solution was slowly added to the dye solution. The reaction was allowed to proceed for 1/2 hour, with occasional shaking. The reaction mixture was poured into water (600 mL), and aqueous sodium sulfite was added to discharge the bromine. The aqueous solution was decanted off. The solid was dissolved in methylene chloride, then concentrated, and slowly added to cold methanol, whereupon a solid precipitated.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05663024uspto-grants-1997_09