Reacción #6604

ord-870f165d08ed449088d95aa4882d0671

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooled to room temperature
  2. 2
    Extracciónextracted with ether
  3. 3
    LavadoThe organic phase was washed
  4. 4
    Secadodried over magnesium sulfate
  5. 5
    Otroevaporated under reduced pressure
  6. 6
    OtroRecrystallization of the residue from methanol

Procedimiento

94.0 g (0.5 mol) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene were stirred into 100 ml of chlorosulfonic acid at 20° C. within 30 min. The reaction solution was maintained at 60° C. for 1 hour, cooled to room temperature and then poured into 1.5 l of ice and extracted with ether. The organic phase was washed to neutrality with brine and water, dried over magnesium sulfate and evaporated under reduced pressure. Recrystallization of the residue from methanol yielded 55.0 g of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-sulfonyl chloride of melting point 71°-74° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05248823uspto-grants-1993_09