Reacción #1687634

ord-dddecb71856e4b40b10c34c0a9991333

Ecuación de reacción

N
ammonia
CC(=O)CNC(=O)c1cccnc1
73
CC(=O)CNC(=O)c1cccnc1
N-Acetylmethyl-nicotinamide
S=P12SP3(=S)SP(=S)(S1)SP(=S)(S2)S3
P4S10
C
charcoal
Cc1cnc(-c2cccnc2)s1
5-Methyl-2-(3-pyridyl)-thiazole

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe suspension was refluxed for 4 h
  2. 2
    Filtraciónfiltered
  3. 3
    OtroThe toluene phase was separated
  4. 4
    Extracciónthe aqueous phase extracted with 2×100 ml of toluene
  5. 5
    SecadoThe combined organic phase were dried over MgSO4
  6. 6
    Otroevaporated in vacuo
  7. 7
    Otroleaving a heavy, yellow oil, 88

Procedimiento

To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: USRE036374uspto-grants-1999_11