Reacción #523489

ord-94b724fd7d4a4caa9290a4f968d23952

Ecuación de reacción

N#C[S-].[K+]
potassium thiocyanate
F
hydrofluoric acid
Cc1cccc2ccccc12
α-methylnaphthalene
Cc1ccc(C(N)=S)c2ccccc12
1-methyl-4-thionaphthamide
Rendimiento 97.0%

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONare added
  2. 2
    workup.STIRRINGby stirring with ice
  3. 3
    workup.DISTILLATIONby distilling off the greater part of the hydrofluoric acid in a steel apparatus
  4. 4
    workup.STIRRINGbefore stirring with ice

Procedimiento

At a temperature and in the manner as described in Example 1, 39 g of potassium thiocyanate (0.4 mol) are stirred into 0.3 l of 98% hydrofluoric acid, 47 g of α-methylnaphthalene (0.33 mol) are added, and the mixture is stirred for 4 hours at room temperature. The reaction is then complete. Work-up is possible by stirring with ice, as described in the preceding Examples, or by distilling off the greater part of the hydrofluoric acid in a steel apparatus before stirring with ice. 64 g of 1-methyl-4-thionaphthamide having a melting point of 143° - 145° C are obtained, which corresponds to a yield of 97% of the theoretical yield, relative to α-methyl-naphthalene used.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04008264uspto-grants-1977_02